Bicyclic Bridgehead Phosphoramidite (Briphos) Ligands with Tunable π-Acceptor Ability and Catalytic Activity in the Rhodium-Catalyzed Conjugate Additions.
Lee, Ansoo; Ahn, Seihwan; Kang, Kyungjun; Seo, Min-Seob; Kim, Yeonjoon; Kim, Woo Youn; Kim, Hyunwoo; Organic letters 16 (2014) 5490–5493; doi:10.1021/ol502772m

data_1517945
_publ_section_title
;
 Bicyclic Bridgehead Phosphoramidite (Briphos) Ligands with Tunable
 \p-Acceptor Ability and Catalytic Activity in the Rhodium-Catalyzed
 Conjugate Additions.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5490
_journal_page_last               5493
_journal_paper_doi               10.1021/ol502772m
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C76 H56 Cl2 N4 O8 P4 Rh2, C7 H8'
_chemical_formula_sum            'C83 H64 Cl2 N4 O8 P4 Rh2'
_chemical_formula_weight         1645.98
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.134(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1059(9)
_cell_length_b                   20.1867(17)
_cell_length_c                   17.7321(16)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.34
_cell_volume                     3507.9(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         1.556
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
; 
 Flack x determined using 6850 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         16121
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14887
_reflns_number_total             16121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol502772m_si_003.cif
_cod_data_source_block           d1426
_cod_depositor_comments
'Adding full bibliography for 1517944--1517945.cif.'
_cod_database_code               1517945
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2013-4
_shelx_res_checksum              2071
_shelx_hkl_checksum              5955