Tandem 1,6-addition/cyclization/vinylcyclopropane rearrangement at low temperature under metal-free conditions: an approach to spiro[4.5]cyclohexadienones.
Yuan, Zhenbo; Gai, Kuo; Wu, Youzhi; Wu, Jie; Lin, Aijun; Yao, Hequan; Chemical communications (Cambridge, England) 53 (2017) 3485–3488; doi:10.1039/c7cc00677b

data_7119702
_publ_section_title
;
 Tandem 1,6-addition/cyclization/vinylcyclopropane rearrangement at low
 temperature under metal-free conditions: an approach to
 spiro[4.5]cyclohexadienones.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3485
_journal_page_last               3488
_journal_paper_doi               10.1039/c7cc00677b
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C32 H40 O5'
_chemical_formula_weight         504.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-09 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.659(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.71
_cell_volume                     3035.3(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.882
_exptl_absorpt_coefficient_mu    0.073
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0914
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_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+0.9396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3588
_reflns_number_total             5351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00677b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7119701--7119702.cif.'
_cod_original_cell_volume        3035.4(12)
_cod_database_code               7119702
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              33678
_shelx_hkl_checksum              43835