D2-Symmetric Dirhodium Catalyst Derived from a 1,2,2-Triarylcyclopropanecarboxylate Ligand: Design, Synthesis and Application
Changming Qin; Vyacheslav Boyarskikh; Jørn H. Hansen; Kenneth I. Hardcastle; Djamaladdin G. Musaev; Huw M. L. Davies; Journal of the American Chemical Society 133 (2011) 19198–19204; doi:10.1021/ja2074104

data_4107163
_publ_section_title
;
 D2-Symmetric Dirhodium Catalyst Derived from a
 1,2,2-Triarylcyclopropanecarboxylate Ligand: Design, Synthesis and
 Application
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19198
_journal_page_last               19204
_journal_paper_doi               10.1021/ja2074104
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C94.70 H80.75 Br4 O11.30 Rh2'
_chemical_formula_sum            'C94.7 H80.75 Br4 O11.3 Rh2'
_chemical_formula_weight         1925.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1690(5)
_cell_length_b                   21.4934(6)
_cell_length_c                   24.0740(6)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.02
_cell_measurement_theta_min      3.18
_cell_volume                     9401.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64982
_diffrn_reflns_theta_full        69.59
_diffrn_reflns_theta_max         69.59
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    5.267
_exptl_absorpt_correction_T_max  0.6026
_exptl_absorpt_correction_T_min  0.3621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             3877
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         2.567
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         16806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+3.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                16077
_reflns_number_total             16806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2074104_si_002.cif
_cod_data_source_block           qin_3_27
_cod_original_formula_sum        'C94.70 H80.75 Br4 O11.30 Rh2'
_cod_database_code               4107163