Lewis Acid activation of carbodicarbene catalysts for rh-catalyzed hydroarylation of dienes.
Roberts, Courtney C.; Matías, Desirée M; Goldfogel, Matthew J.; Meek, Simon J.; Journal of the American Chemical Society 137 (2015) 6488–6491; doi:10.1021/jacs.5b03510

data_4123649
_publ_section_title
;
 Lewis Acid activation of carbodicarbene catalysts for rh-catalyzed
 hydroarylation of dienes.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6488
_journal_page_last               6491
_journal_paper_doi               10.1021/jacs.5b03510
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C41 H39.2 N4 P2 Rh, C32 H12 B F23.89'
_chemical_formula_sum            'C73 H52 B F24 N4 P2 Rh'
_chemical_formula_weight         1616.85
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_cell_angle_alpha                72.9946(16)
_cell_angle_beta                 69.1536(17)
_cell_angle_gamma                78.1710(16)
_cell_formula_units_Z            2
_cell_length_a                   14.5732(5)
_cell_length_b                   16.2543(6)
_cell_length_c                   16.4636(6)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    100(2)
_cell_volume                     3462.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54146
_diffrn_reflns_theta_full        70.15
_diffrn_reflns_theta_max         70.15
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.427
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0530 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.8805.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.193
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         12784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                12172
_reflns_number_total             12784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b03510_si_002.cif
_cod_data_source_block           x1411004
_cod_depositor_comments          'Adding full bibliography for 4123649.cif.'
_cod_database_code               4123649
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) = Uanis(C43)
Uanis(C40) = Uanis(C42)
3. Others
 Sof(C43)=1-FVAR(1)
 Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
 Sof(C42)=1-FVAR(2)
 Sof(C40)=Sof(H40)=FVAR(2)
 Sof(F9A)=Sof(F7A)=Sof(F8A)=1-FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(3)
 Sof(F18A)=Sof(F17A)=Sof(F16A)=1-FVAR(4)
 Sof(F18)=Sof(F16)=Sof(F17)=FVAR(4)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(5)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(5)
4.a Ternary CH refined with riding coordinates:
 C40(H40)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C23(H23), C15(H15), C14(H14), C13(H13), C12(H12), C26(H26),
 C27(H27), C29(H29), C33(H33), C30(H30), C24(H24), C25(H25), C57(H57), C53(H53),
  C55(H55), C31(H31), C32(H32), C17(H17), C21(H21), C19(H19), C18(H18),
 C73(H73), C71(H71), C69(H69), C61(H61), C65(H65), C63(H63), C49(H49), C45(H45),
  C47(H47), C20(H20), C35(H35), C36(H36), C39(H39), C38(H38), C37(H37)
4.d X=CH2 refined with riding coordinates:
 C41(H41A,H41B)
;
_olex2_submission_special_instructions 'No special instructions were received'