(4+1) vs (4+2): Catalytic Intramolecular Coupling between Cyclobutanones and Trisubstituted Allenes via C-C Activation.
Zhou, Xuan; Dong, Guangbin; Journal of the American Chemical Society 137 (2015) 13715–13721; doi:10.1021/jacs.5b09799

data_4129704
_publ_section_title
;
 (4+1) vs (4+2): Catalytic Intramolecular Coupling between Cyclobutanones
 and Trisubstituted Allenes via C-C Activation.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13715
_journal_page_last               13721
_journal_paper_doi               10.1021/jacs.5b09799
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C22 H29 N O3 S'
_chemical_formula_sum            'C22 H29 N O3 S'
_chemical_formula_weight         387.52
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_space_group_name_Hall           '-P 2yn'
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_cell_length_c                   30.223(3)
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_cell_measurement_temperature    133(2)
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_cell_measurement_theta_min      2.1
_cell_volume                     4068.1(7)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
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_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
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_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       \w-scans
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_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_min       -36
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.364
_diffrn_reflns_theta_min         0.681
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS.
;
_exptl_crystal_colour            colorless
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_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
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_exptl_crystal_size_min          0.098
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_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.359
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+3.7348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1995
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
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_reflns_number_total             7426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09799_si_006.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129704
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4
_shelx_res_checksum              10151
_shelx_hkl_checksum              69482