Construction of Rhodium(I) and Gold(I) Macrocycles by Transferring a Phosphine-Functionalized 4,5-Diazafluorenide Ligand from Its Copper(I) N-Heterocyclic Carbene Complex
Tan, Runyu; Chiu, Frederick Sin Nang; Hadzovic, Alen; Song, Datong; Organometallics 31 (2012) 2184–; doi:10.1021/om200994b

data_4076345
_publ_section_title
;
 Construction of Rhodium(I) and Gold(I) Macrocycles by Transferring a
 Phosphine-Functionalized 4,5-Diazafluorenide Ligand from Its Copper(I)
 N-Heterocyclic Carbene Complex
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2184
_journal_paper_doi               10.1021/om200994b
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C64 H80 Au N4 O3 P'
_chemical_formula_weight         1181.26
_chemical_name_systematic
; 
 ? 
;
_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                 104.265(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1203(8)
_cell_length_b                   15.9161(6)
_cell_length_c                   18.5991(7)
_cell_measurement_reflns_used    13202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      1.71
_cell_volume                     5772.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50003
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.8175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'bruker apex 2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.855
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         13202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+6.3697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                10089
_reflns_number_total             13202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200994b_si_001.cif
_cod_data_source_block           2f
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4076345