Silver-Catalyzed Cascade 1,6-Addition/Cyclization of para-Quinone Methides with Propargyl Malonates: An Approach to Spiro[4.5]deca-6,9-dien-8-ones.
Yuan, Zhenbo; Liu, Lina; Pan, Rui; Yao, Hequan; Lin, Aijun; The Journal of organic chemistry 82 (2017) 8743–8751; doi:10.1021/acs.joc.7b01400

data_4032816
_publ_section_title
;
 Silver-Catalyzed Cascade 1,6-Addition/Cyclization of para-Quinone
 Methides with Propargyl Malonates: An Approach to
 Spiro[4.5]deca-6,9-dien-8-ones.
;
_journal_issue                   16
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8743
_journal_page_last               8751
_journal_paper_doi               10.1021/acs.joc.7b01400
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C29 H36 O5'
_chemical_formula_weight         464.58
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
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_cell_angle_gamma                90
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_cell_length_b                   30.750(14)
_cell_length_c                   15.411(7)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      45.035
_cell_measurement_theta_min      2.226
_cell_volume                     5388(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker samrt CCD'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37053
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         1.324
_exptl_absorpt_coefficient_mu    0.077
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0030(6)
_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   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         9340
_refine_ls_number_restraints     1028
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0910P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5200
_reflns_number_total             9340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01400_si_002.cif
_cod_data_source_block           a
_cod_database_code               4032816
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-2
_shelx_res_checksum              20223
_shelx_hkl_checksum              68518