Photochemical Disproportionation of an AuIIPincer Complex: Synthesis and Structure of an AuI4AuIII4Macrocycle
Roşca, Dragoş-Adrian; Bochmann, Manfred; Organometallics 35 (2015) 27–; doi:10.1021/acs.organomet.5b00846

data_4088109
_publ_section_title
;
 Photochemical Disproportionation of an AuIIPincer Complex: Synthesis and
 Structure of an AuI4AuIII4Macrocycle
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              27
_journal_paper_doi               10.1021/acs.organomet.5b00846
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C50 H54 Au2 N2, 2(C6 H6)'
_chemical_formula_sum            'C62 H66 Au2 N2'
_chemical_formula_weight         1233.11
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 121.135(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.609(2)
_cell_length_b                   26.9775(15)
_cell_length_c                   17.476(2)
_cell_measurement_reflns_used    8956
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      0.748
_cell_measurement_theta_min      0.713
_cell_volume                     5088.3(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68930
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    5.798
_exptl_absorpt_correction_T_max  0.7603
_exptl_absorpt_correction_T_min  0.4767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.812
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8940
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+11.4460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                7818
_reflns_number_total             8940
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00846_si_001.cif
_cod_data_source_block           dragos51
_cod_original_cell_volume        5088.3(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4088109