Tuning the Chiral Environment ofC2-Symmetric Diene Ligands: Development of 3,7-Disubstituted Bicyclo[3.3.1]nona-2,6-dienes
Ryo Shintani; Yoshitaka Ichikawa; Keishi Takatsu; Fu-Xue Chen; Tamio Hayashi; Journal of Organic Chemistry 74 (2009) 869–873; doi:10.1021/jo802437h

data_4024279
_publ_section_title
;
Tuning the Chiral Environment ofC2-Symmetric Diene Ligands: Development of
3,7-Disubstituted Bicyclo[3.3.1]nona-2,6-dienes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              869
_journal_page_last               873
_journal_paper_doi               10.1021/jo802437h
_journal_volume                  74
_journal_year                    2009
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C42 H40 Cl2 Rh2 '
_chemical_formula_sum            'C42 H40 Cl2 Rh2'
_chemical_formula_weight         821.50
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.989(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.314(4)
_cell_length_b                   15.290(4)
_cell_length_c                   18.582(6)
_cell_measurement_reflns_used    32128
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3395.0(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32857
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.12
_refine_diff_density_min         -1.23
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6754 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.017(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         31369
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.0071
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    40.7586    24.5053    7.8147
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0285
_reflns_number_gt                31322
_reflns_number_total             14809
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo802437h_si_001.cif
_cod_data_source_block           '_71002yuki'
_cod_original_formula_sum        'C42 H40 Cl2 Rh2 '
_cod_database_code               4024279