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_4119989
_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         'C56 H64 Ag2 N8, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C60 H70 Ag2 F12 N10 P2'
_chemical_formula_weight         1436.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                102.6720(10)
_cell_angle_beta                 109.0550(10)
_cell_angle_gamma                111.0600(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7685(2)
_cell_length_b                   12.2958(2)
_cell_length_c                   13.1428(2)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.34706
_cell_measurement_theta_min      2.5955
_cell_volume                     1550.51(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22567
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.8605
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 numerical correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0596P)^2^+2.2504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                7844
_reflns_number_total             8980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4032067_si_002.cif
_cod_data_source_block           structureneu
_cod_original_cell_volume        1550.51(4)
_cod_database_code               4119989