Chiral Crown Conformation of Rh2(S-PTTL)4: Enantioselective Cyclopropanation with α-Alkyl-α-diazoesters
Andrew DeAngelis; Olga Dmitrenko; Glenn P. A. Yap; Joseph M. Fox; Journal of the American Chemical Society 131 (2009) 7230–7231; doi:10.1021/ja9026852

data_4104460
_publ_section_title
;
 Chiral Crown Conformation of Rh2(S-PTTL)4: Enantioselective
 Cyclopropanation with \a-Alkyl-\a-diazoesters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7230
_journal_page_last               7231
_journal_paper_doi               10.1021/ja9026852
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C78 H88 N4 O20 Rh2'
_chemical_formula_weight         1607.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.456(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.182(4)
_cell_length_b                   20.088(6)
_cell_length_c                   28.868(9)
_cell_measurement_reflns_used    997
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      16.22
_cell_measurement_theta_min      2.15
_cell_volume                     8172(4)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.1366
_diffrn_reflns_av_sigmaI/netI    0.1998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81795
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
Void space analysis consistent with initial solutions displaying
four toluene molecules and two ethylacetate molecules 
cocrystallized and severly disordered  in the asymmetric 
unit todether with with two symmetry-unique compound molecules.
;
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881: 13930 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         28757
_refine_ls_number_restraints     813
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                15266
_reflns_number_total             28757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9026852_si_001.cif
_cod_data_source_block           joef082s
_cod_database_code               4104460