Synthesis of allene triazole through iron catalyzed regioselective addition to propargyl alcohols
Wuming Yan; Xiaohan Ye; Keith Weise; Jeffrey L. Petersen; Xiaodong Shi; Chem.Commun. 48 (2012) 3521–; doi:10.1039/c2cc17522c

data_7107501
_publ_section_title
;
 Synthesis of allene triazole through iron catalyzed regioselective
 addition to propargyl alcohols
;
_journal_name_full               Chem.Commun.
_journal_page_first              3521
_journal_paper_doi               10.1039/c2cc17522c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C27 H26 N6 Si'
_chemical_formula_weight         462.63
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.773(2)
_cell_angle_beta                 92.532(2)
_cell_angle_gamma                96.523(2)
_cell_formula_units_Z            4
_cell_length_a                   12.0515(12)
_cell_length_b                   15.0765(15)
_cell_length_c                   15.9874(16)
_cell_measurement_temperature    293(2)
_cell_volume                     2606.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18732
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9530
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         11679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0921P)^2^+0.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2013
_reflns_number_gt                6972
_reflns_number_total             11679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc17522c.txt
_cod_data_source_block           xs40ccd
_cod_database_code               7107501