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_7119701
_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            'C30 H36 Cl N0 O5'
_chemical_formula_weight         512.04
_chemical_name_systematic
'diethyl 7,9-di-tert-butyl-4-(4-chlorophenyl)-8-oxospiro[4.5]deca-2,6,9-triene-1,1-dicarboxylate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1k3w3n
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-28 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.910(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7421(6)
_cell_length_b                   16.0093(9)
_cell_length_c                   19.0370(11)
_cell_measurement_reflns_used    6590
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.27
_cell_volume                     2958.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20847
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_correction_T_min  0.9557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/n-hexane'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.053(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0856P)^2^+1.3051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1870
_reflns_number_gt                3468
_reflns_number_total             5212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00677b2.cif
_cod_data_source_block           20151014zy_gk_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7119701--7119702.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7119701