Irradiation-Induced Heck Reaction of Unactivated Alkyl Halides at Room Temperature.
Wang, Guang-Zu; Shang, Rui; Cheng, Wan-Min; Fu, Yao; Journal of the American Chemical Society 139 (2017) 18307–18312; doi:10.1021/jacs.7b10009

data_4131748
_publ_section_title
;
 Irradiation-Induced Heck Reaction of Unactivated Alkyl Halides at Room
 Temperature.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18307
_journal_page_last               18312
_journal_paper_doi               10.1021/jacs.7b10009
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C36 H54 O'
_chemical_formula_weight         502.79
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.0050(10)
_cell_angle_beta                 87.5840(10)
_cell_angle_gamma                89.6900(10)
_cell_formula_units_Z            2
_cell_length_a                   7.73350(10)
_cell_length_b                   14.1534(2)
_cell_length_c                   14.5834(2)
_cell_measurement_reflns_used    30955
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.2500
_cell_measurement_theta_min      5.7140
_cell_volume                     1553.95(4)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2015)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 5.2169
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41658
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.329
_diffrn_reflns_theta_min         3.935
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 4626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.06(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11228
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0969P)^2^+0.0952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.907
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                10314
_reflns_number_total             11228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10009_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4131748
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.906
_shelxl_version_number           2013-4
_shelx_res_checksum              21449
_shelx_hkl_checksum              11451