Gold-Mediated Expulsion of Dinitrogen from Organic Azides
Chandrakanta Dash; Muhammed Yousufuddin; Thomas R. Cundari; H. V. Rasika Dias; Journal of the American Chemical Society 135 (2013) 15479–15488; doi:10.1021/ja406027x

data_4120932
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
The University of Texas at Arlington
700 Planetarium Place, Room 130 CPB
Arlington, Texas 76019-0065, USA
;
_publ_contact_author_email       dias@uta.edu
_publ_contact_author_fax         817-272-3808
_publ_contact_author_name        'Rasika Dias'
_publ_contact_author_phone       817-272-3813
_publ_section_title
;
 Gold-Mediated Expulsion of Dinitrogen from Organic Azides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15479
_journal_page_last               15488
_journal_paper_doi               10.1021/ja406027x
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C37 H53 Au N5, F6 Sb'
_chemical_formula_sum            'C37 H53 Au F6 N5 Sb'
_chemical_formula_weight         1000.56
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.982(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7961(8)
_cell_length_b                   16.7771(13)
_cell_length_c                   12.9004(10)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.63
_cell_measurement_theta_min      3.24
_cell_volume                     1979.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29485
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    4.444
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.048
_refine_diff_density_max         3.156
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
; 
 Flack x determined using 4630 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.084(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         11940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0138P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                10771
_reflns_number_total             11940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406027x_si_002_6.cif
_cod_data_source_block           rad7
_cod_database_code               4120932
_shelxl_version_number           2013-2