Tandem indole C-H alkenylation/arylation for tetra-substituted alkene synthesis
Laura Lopez-Suarez; Michael F. Greaney; Chem.Commun. 47 (2011) 7992–; doi:10.1039/c1cc13094c

data_7106659
_publ_section_title
;
 Tandem indole C-H alkenylation/arylation for tetra-substituted alkene
 synthesis
;
_journal_name_full               Chem.Commun.
_journal_page_first              7992
_journal_paper_doi               10.1039/c1cc13094c
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'Laura Lopez'
_chemical_formula_moiety         'C27 H25 N'
_chemical_formula_sum            'C27 H25 N'
_chemical_formula_weight         363.48
_space_group_IT_number           15
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_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.899(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.1976(8)
_cell_length_b                   5.64047(14)
_cell_length_c                   19.7426(4)
_cell_measurement_reflns_used    6644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.3505
_cell_measurement_theta_min      2.2412
_cell_volume                     3910.45(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
1 omega -107.00 -18.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -39.8164 -37.0000 -30.0000 89

2 omega -101.00 -14.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -39.8164 -37.0000 -120.0000 87

3 omega 37.00 74.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 -60.0000 37

4 omega 94.00 172.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -120.0000 78

5 omega 32.00 64.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 120.0000 32

6 omega 45.00 91.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -112.0000 144.0000 46

7 omega 84.00 163.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -60.0000 79

8 omega 43.00 76.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 -30.0000 33

9 omega 83.00 127.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -150.0000 44

10 omega 144.00 175.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 125.0000 120.0000 31

11 omega 111.00 178.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 125.0000 -180.0000 67

12 omega -119.00 -6.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -39.8164 -77.0000 150.0000 113

13 omega 56.00 130.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 39.8164 179.0000 30.0000 74

14 omega -140.00 -28.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -61.5000 -77.0000 90.0000 112

15 omega 24.00 169.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -15.0000 150.0000 145

16 omega 80.00 178.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -180.0000 98

17 omega 32.00 77.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 60.0000 45

18 omega 46.00 178.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 15.0000 60.0000 132

19 omega 28.00 141.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 -77.0000 -180.0000 113

20 omega -119.00 -6.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -39.8164 -77.0000 -120.0000 113

21 omega 56.00 130.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 39.8164 179.0000 -180.0000 74

22 omega -140.00 -28.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -61.5000 -77.0000 0.0000 112

23 omega 74.00 167.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 107.1667 77.0000 90.0000 93

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20314
_diffrn_reflns_theta_full        73.51
_diffrn_reflns_theta_max         73.51
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method
'vapour diffusion of hexane into toluene solution'
_exptl_crystal_size_max          0.1752
_exptl_crystal_size_mid          0.0658
_exptl_crystal_size_min          0.0302
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                2750
_reflns_number_total             3864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13094c.txt
_cod_data_source_block           mg0011
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7106659