1,3-Carboboration of iodonium ylides.
Gazis, Theodore A.; Mohajeri Thaker, Bayan A. J.; Willcox, Darren; Ould, Darren M. C.; Wenz, Jan; Rawson, Jeremy M.; Hill, Michael S.; Wirth, Thomas; Melen, Rebecca L.; Chemical communications (Cambridge, England) 56 (2020) 3345–3348; doi:10.1039/c9cc08749d

data_7126008
_publ_section_title
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 1,3-Carboboration of iodonium ylides.
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_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3345
_journal_page_last               3348
_journal_paper_doi               10.1039/c9cc08749d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C33 H16 B F9 O2'
_chemical_formula_sum            'C33 H16 B F9 O2'
_chemical_formula_weight         626.27
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-16
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-12-05 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                85.283(4)
_cell_angle_beta                 75.672(4)
_cell_angle_gamma                66.463(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7170(4)
_cell_length_b                   10.2493(5)
_cell_length_c                   15.4586(9)
_cell_measurement_reflns_used    3929
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      28.1280
_cell_measurement_theta_min      4.0230
_cell_volume                     1367.33(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5082
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  71.00   1.00   24.88    --   10.74  57.00   0.00   88
  2  \w    -77.00  12.00   1.00   24.88    --  -11.13 -57.00  60.00   89
  3  \w    -37.00  62.00   1.00   24.88    --  -11.13  57.00-150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0071977000
_diffrn_orient_matrix_UB_12      -0.0278295000
_diffrn_orient_matrix_UB_13      -0.0421608000
_diffrn_orient_matrix_UB_21      0.0517571000
_diffrn_orient_matrix_UB_22      0.0326731000
_diffrn_orient_matrix_UB_23      -0.0203875000
_diffrn_orient_matrix_UB_31      0.0630792000
_diffrn_orient_matrix_UB_32      -0.0621121000
_diffrn_orient_matrix_UB_33      0.0070904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.635
_diffrn_reflns_theta_min         3.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
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            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/pentane'
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0474
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4319
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08749d2.cif
_cod_data_source_block           rm1919
_cod_depositor_comments
'Adding full bibliography for 7126008--7126012.cif.'
_cod_database_code               7126008
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              84746
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.809
_publcif_funding_html
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;