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_7106660
_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 O'
_chemical_formula_sum            'C27 H25 N O'
_chemical_formula_weight         379.48
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_cell_angle_beta                 102.2682(18)
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_cell_formula_units_Z            8
_cell_length_a                   38.3667(7)
_cell_length_b                   5.55996(10)
_cell_length_c                   18.9626(3)
_cell_measurement_reflns_used    10691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4116
_cell_measurement_theta_min      2.3551
_cell_volume                     3952.68(12)
_computing_cell_refinement
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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_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
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_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
1 omega -66.00 21.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 37.0000 60.0000 87

2 omega -110.00 -14.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 -37.0000 -120.0000 96

3 omega -59.00 -34.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 179.0000 90.0000 25

4 omega 49.00 77.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 30.0000 28

5 omega 32.00 72.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 -90.0000 40

6 omega 88.00 176.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -150.0000 88

7 omega 70.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 15.0000 150.0000 108

8 omega 30.00 118.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -77.0000 -150.0000 88

9 omega 118.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 125.0000 120.0000 60

10 omega -119.00 -7.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 -77.0000 90.0000 112

11 omega 56.00 130.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.1914 179.0000 -90.0000 74

12 omega 80.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -30.0000 98

13 omega 32.00 77.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 90.0000 45

14 omega 30.00 116.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -113.0000 117.0000 86

15 omega 80.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 60.0000 98

16 omega -119.00 -7.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 -77.0000 0.0000 112

17 omega -119.00 -7.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.1914 -77.0000 -180.0000 112

18 omega 80.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 45.0000 -90.0000 98

19 omega 74.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 77.0000 0.0000 104

20 omega 74.00 178.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 77.0000 150.0000 104

21 omega 32.00 77.00 1.0000 4.0800
omega____ theta____ kappa____ phi______ frames
- 107.1667 -45.0000 -30.0000 45

22 omega 56.00 87.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.1914 179.0000 0.0000 31

;
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19039
_diffrn_reflns_theta_full        73.57
_diffrn_reflns_theta_max         73.57
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83834
_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    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method 'slow evaporation of DCM/MeNO2 solution'
_exptl_crystal_size_max          0.1506
_exptl_crystal_size_mid          0.1271
_exptl_crystal_size_min          0.0448
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0899P)^2^+0.7030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                3311
_reflns_number_total             3918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13094c.txt
_cod_data_source_block           mg0012
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7106660