Copper-catalyzed trans-carbohalogenation of terminal alkynes with functionalized tertiary alkyl halides.
Che, Chao; Zheng, Hanliang; Zhu, Gangguo; Organic letters 17 (2015) 1617–1620; doi:10.1021/acs.orglett.5b00546

data_1554875
_publ_section_title
;
 Copper-catalyzed trans-carbohalogenation of terminal alkynes with
 functionalized tertiary alkyl halides.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1617
_journal_page_last               1620
_journal_paper_doi               10.1021/acs.orglett.5b00546
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C12 H13 Br O2'
_chemical_formula_weight         269.13
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
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_cell_angle_beta                 97.594(3)
_cell_angle_gamma                90
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_cell_length_b                   11.7969(15)
_cell_length_c                   16.772(2)
_cell_measurement_reflns_used    2274
_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      4.900
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0466
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_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.117
_exptl_absorpt_coefficient_mu    3.467
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4639
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_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prismatic
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.123
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_refine_ls_extinction_coef       0.0191(16)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1907
_reflns_number_total             2320
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           cd214519
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1554875
_shelxl_version_number           2013-4
_shelx_res_checksum              85197
_shelx_hkl_checksum              35987