Postsynthetic Modification of Dicarbene-Derived Metallacycles via Photochemical [2 + 2] Cycloaddition
Ying-Feng Han; Guo-Xin Jin; F. Ekkehardt Hahn; Journal of the American Chemical Society 135 (2013) 9263–9266; doi:10.1021/ja4032067

data_4119990
_publ_section_title
;
 Postsynthetic Modification of Dicarbene-Derived Metallacycles via
 Photochemical [2 + 2] Cycloaddition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9263
_journal_page_last               9266
_journal_paper_doi               10.1021/ja4032067
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C48 H48 Au2 N8, 2(Cl O4)'
_chemical_formula_sum            'C48 H48 Au2 Cl2 N8 O8'
_chemical_formula_weight         1329.78
_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                 100.183(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0716(4)
_cell_length_b                   41.7167(17)
_cell_length_c                   14.2731(6)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.4195
_cell_measurement_theta_min      2.7105
_cell_volume                     5316.4(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            94759
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         32.12
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    5.670
_exptl_absorpt_correction_T_max  0.3968
_exptl_absorpt_correction_T_min  0.3968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.487
_refine_diff_density_min         -4.207
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         17164
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+41.8727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                12702
_reflns_number_total             17164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4032067_si_003.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4119990