Pathways to Functionalized Heterocycles: Propargyl Rearrangement using B(C6F5)3
Wilkins, Lewis C.; Wieneke, Philipp; Newman, Paul D.; Kariuki, Benson M.; Rominger, Frank; Hashmi, A. Stephen K.; Hansmann, Max M.; Melen, Rebecca L.; Organometallics 34 (2015) 5298–; doi:10.1021/acs.organomet.5b00753

data_4087967
_publ_section_title
;
 Pathways to Functionalized Heterocycles: Propargyl Rearrangement using
 B(C6F5)3
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5298
_journal_paper_doi               10.1021/acs.organomet.5b00753
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H12 B F15 O3'
_chemical_formula_sum            'C26 H12 B F15 O3'
_chemical_formula_weight         668.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                96.542(3)
_cell_angle_beta                 91.236(3)
_cell_angle_gamma                97.100(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6463(4)
_cell_length_b                   12.1922(5)
_cell_length_c                   12.2500(5)
_cell_measurement_reflns_used    5266
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.027
_cell_measurement_theta_min      3.914
_cell_volume                     1419.43(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'SuperNova Dual Atlas with CCD plate'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13624
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.916
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'SuperNova (Mo) X-ray source'
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.989
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model. Empirical absorption correction using 
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.3075
_exptl_crystal_size_mid          0.2129
_exptl_crystal_size_min          0.0792
_platon_squeeze_details
;
TITL rm15104   P -1         R = 0.12
CELL    9.6463   12.1922   12.2500     96.54     91.24     97.10
SPGR P-1
C101 0.988 0.997 0.412 !       5.85 eA-3
C102 0.160 0.894 0.471 !       4.26 eA-3
C103 0.070 0.936 0.396 !       3.69 eA-3
C104 0.080 0.956 0.487 !       3.62 eA-3
C105 0.904 0.060 0.420 !       3.00 eA-3
;
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0444P)^2^+0.8022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4921
_reflns_number_total             6742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00753_si_014.cif
_cod_data_source_block           rm15104_sq
_cod_database_code               4087967
_shelxl_version_number           2013-3
_shelx_res_checksum              34496
_shelx_hkl_checksum              32231
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              70487