A palladium-catalyzed tandem reaction of 2-(2-bromobenzylidene)cyclobutanone with 2-alkynylphenol.
Pan, Xiaolin; Luo, Yong; Xia, Hong-Guang; Wu, Jie; Chemical communications (Cambridge, England) 51 (2015) 16483–16485; doi:10.1039/c5cc07360j

data_7118037
_publ_section_title
;
 A palladium-catalyzed tandem reaction of
 2-(2-bromobenzylidene)cyclobutanone with 2-alkynylphenol.
;
_journal_issue                   92
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16483
_journal_page_last               16485
_journal_paper_doi               10.1039/c5cc07360j
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C25 H18 O2'
_chemical_formula_weight         350.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-08-27 deposited with the CCDC.
2015-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                77.278(10)
_cell_angle_beta                 70.928(9)
_cell_angle_gamma                88.102(9)
_cell_formula_units_Z            2
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_cell_length_b                   9.320(8)
_cell_length_c                   11.404(9)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.62
_cell_volume                     908.9(13)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.962
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_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4264
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         1.938
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.020(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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0937P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2171
_reflns_number_total             3119
_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_estimated_absorpt_t_min   0.969
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_shelxl_version_number           2013-2
_shelx_res_checksum              73879