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_4120931
_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
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_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
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 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_formula_moiety         'C38 H57 Au N3 O, F6 Sb, C H2 Cl2'
_chemical_formula_sum            'C39 H59 Au Cl2 F6 N3 O Sb'
_chemical_formula_weight         1089.51
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2013-05-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                96.960(1)
_cell_angle_beta                 102.634(1)
_cell_angle_gamma                114.233(1)
_cell_formula_units_Z            2
_cell_length_a                   12.3193(6)
_cell_length_b                   12.4746(6)
_cell_length_c                   16.1379(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.75
_cell_measurement_theta_min      2.30
_cell_volume                     2143.84(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.86
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.232
_exptl_absorpt_correction_T_max  0.7123
_exptl_absorpt_correction_T_min  0.3445
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.864
_refine_diff_density_min         -2.595
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         15899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                13531
_reflns_number_total             15899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406027x_si_002_5.cif
_cod_data_source_block           dias962_0m_a
_cod_database_code               4120931
_olex2_refinement_description
;
1. others
 Fixed Uiso: H2A(0.021) H2B(0.021) H3A(0.022) H3B(0.022) H6(0.024) H7(0.026)
 H8(0.023) H10(0.021) H11A(0.047) H11B(0.047) H11C(0.047) H12A(0.052)
 H12B(0.052) H12C(0.052) H13(0.02) H14A(0.044) H14B(0.044) H14C(0.044)
 H15A(0.049) H15B(0.049) H15C(0.049) H18(0.022) H19(0.024) H20(0.023)
 H22(0.023) H23A(0.037) H23B(0.037) H23C(0.037) H24A(0.042) H24B(0.042)
 H24C(0.042) H25(0.022) H26A(0.042) H26B(0.042) H26C(0.042) H27A(0.054)
 H27B(0.054) H27C(0.054) H29A(0.025) H29B(0.025) H30A(0.028) H30B(0.028)
 H31A(0.025) H31B(0.025) H32(0.025) H33A(0.029) H33B(0.029) H34(0.029)
 H35A(0.037) H35B(0.037) H36(0.036) H37A(0.035) H37B(0.035) H38A(0.042)
 H38B(0.042) H38C(0.042) H39A(0.042) H39B(0.042)
 Fixed X: H2A(1.2006) H2B(1.1397) H3A(1.2236) H3B(1.2729) H6(0.892) H7(0.7448)
 H8(0.7279) H10(1.1145) H11A(1.1807) H11B(1.2116) H11C(1.0956) H12A(0.9407)
 H12B(1.0622) H12C(0.9518) H13(0.8993) H14A(0.8007) H14B(0.8557) H14C(0.9464)
 H15A(0.6924) H15B(0.697) H15C(0.6461) H18(1.2071) H19(1.1365) H20(1.0449)
 H22(1.1801) H23A(1.376) H23B(1.3778) H23C(1.384) H24A(1.0573) H24B(1.1773)
 H24C(1.174) H25(0.9723) H26A(1.1562) H26B(1.1738) H26C(1.0785) H27A(0.9411)
 H27B(0.8688) H27C(0.8413) H29A(0.5849) H29B(0.6289) H30A(0.7331) H30B(0.7455)
 H31A(0.5418) H31B(0.6146) H32(0.3955) H33A(0.3146) H33B(0.404) H34(0.4143)
 H35A(0.407) H35B(0.5327) H36(0.5799) H37A(0.5357) H37B(0.4096) H38A(0.784)
 H38B(0.9266) H38C(0.8259) H39A(0.6221) H39B(0.4836)
 Fixed Y: H2A(0.4894) H2B(0.3885) H3A(0.2795) H3B(0.374) H6(0.6328) H7(0.5726)
 H8(0.4198) H10(0.5172) H11A(0.7181) H11B(0.7151) H11C(0.7374) H12A(0.5528)
 H12B(0.5453) H12C(0.4293) H13(0.2438) H14A(0.3393) H14B(0.2448) H14C(0.3805)
 H15A(0.149) H15B(0.1029) H15C(0.2004) H18(0.1519) H19(-0.0518) H20(-0.1238)
 H22(0.3769) H23A(0.3636) H23B(0.4859) H23C(0.3896) H24A(0.3086) H24B(0.4347)
 H24C(0.3111) H25(0.0422) H26A(-0.0458) H26B(0.0834) H26C(-0.0374) H27A(-
 0.1944) H27B(-0.1634) H27C(-0.1468) H29A(-0.0493) H29B(0.0388) H30A(0.3063)
 H30B(0.292) H31A(0.0509) H31B(0.193) H32(0.0931) H33A(-0.0142) H33B(-0.0693)
 H34(-0.0331) H35A(0.1544) H35B(0.1707) H36(0.3325) H37A(0.2958) H37B(0.2323)
 H38A(-0.0138) H38B(0.0729) H38C(0.0156) H39A(0.7287) H39B(0.7052)
 Fixed Z: H2A(0.6831) H2B(0.5919) H3A(0.6568) H3B(0.75) H6(0.7408) H7(0.6045)
 H8(0.4957) H10(0.8019) H11A(0.7832) H11B(0.8843) H11C(0.8397) H12A(0.8793)
 H12B(0.9326) H12C(0.8615) H13(0.5228) H14A(0.3894) H14B(0.3745) H14C(0.4302)
 H15A(0.532) H15B(0.4364) H15C(0.4525) H18(0.9796) H19(0.9147) H20(0.764)
 H22(0.869) H23A(0.9948) H23B(0.9727) H23C(0.9011) H24A(0.9636) H24B(1.0124)
 H24C(1.0325) H25(0.6143) H26A(0.6253) H26B(0.6085) H26C(0.535) H27A(0.6285)
 H27B(0.5472) H27C(0.639) H29A(0.8644) H29B(0.9586) H30A(0.8558) H30B(0.9538)
 H31A(0.6511) H31B(0.6924) H32(0.6797) H33A(0.7707) H33B(0.7482) H34(0.901)
 H35A(0.9204) H35B(0.9878) H36(0.9177) H37A(0.7642) H37B(0.7898) H38A(0.9239)
 H38B(0.9334) H38C(0.8388) H39A(0.5745) H39B(0.5256)
;