Regioselective 1,3-Dipolar Cycloaddition Reaction of Azides with Alkoxy Alkynyl Fischer Carbene Complexes
Chakraborty, Amarnath; Dey, Surjendu; Sawoo, Sudeshna; Adarsh, N. N.; Sarkar, Amitabha; Organometallics 29 (2010) 6619–; doi:10.1021/om1009523

data_4067235
_publ_section_title
;
 Regioselective 1,3-Dipolar Cycloaddition Reaction of Azides with Alkoxy
 Alkynyl Fischer Carbene Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6619
_journal_paper_doi               10.1021/om1009523
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C23 H17 N3 O6 W'
_chemical_formula_weight         615.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 94.111(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   39.965(5)
_cell_length_b                   24.458(3)
_cell_length_c                   18.510(2)
_cell_measurement_temperature    100(2)
_cell_volume                     18046(4)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84054
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    5.165
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.2888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9536
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.494(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1931
_refine_ls_number_reflns         31715
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                22838
_reflns_number_total             31715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009523_si_002.cif
_cod_data_source_block           amar1_0m
_cod_original_cell_volume        18047(4)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4067235