Entrapment of a Dirhodium Tetracarboxylate Unit Inside the Aromatic Bowl of a Calix[4]arene: Unique Catalysts for C-H Amination
J.Du Bois; B.H.Brodsky; Chemical Communications  (2006) –; doi:10.1039/b611280c

data_7101548
_publ_section_title
;
Entrapment of a Dirhodium Tetracarboxylate Unit Inside
the Aromatic Bowl of a Calix[4]arene: Unique Catalysts for C-H
Amination
;
_journal_issue                   45
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b611280c
_journal_year                    2006
_chemical_formula_moiety         'C56 H65 F3 O20 Rh2, C4 H10 O'
_chemical_formula_sum            'C60 H75 F3 O21 Rh2'
_chemical_formula_weight         1395.02
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                86.286(2)
_cell_angle_beta                 88.553(2)
_cell_angle_gamma                86.249(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1442(11)
_cell_length_b                   15.8470(16)
_cell_length_c                   17.7174(17)
_cell_measurement_reflns_used    3286
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.56
_cell_volume                     3115.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20750
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G.M. Sheldrick (1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         12496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                7942
_reflns_number_total             12496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611280c.txt
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101548