H2activation using the first 1 : 1 : 1 hetero-tri(aryl)borane
Blagg, Robin J.; Wildgoose, Gregory G.; RSC Adv. 6 (2016) 42421–; doi:10.1039/C6RA07007H

data_7225036
_publ_section_title
;
 H2activation using the first 1&#x2009;:&#x2009;1&#x2009;:&#x2009;1
 hetero-tri(aryl)borane
;
_journal_issue                   48
_journal_name_full               'RSC Adv.'
_journal_page_first              42421
_journal_paper_doi               10.1039/C6RA07007H
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C20 H3 B Cl5 F11'
_chemical_formula_sum            'C20 H3 B Cl5 F11'
_chemical_formula_weight         640.28
_chemical_name_systematic
(pentafluorophenyl){3,5-bis(trifluoromethyl)phenyl}(pentachlorophenyl)borane
_chemical_properties_physical    Moisture-sensitive
_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
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
;
2016-04-13 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                86.822(8)
_cell_angle_beta                 86.077(9)
_cell_angle_gamma                74.230(10)
_cell_formula_units_Z            4
_cell_length_a                   8.9724(11)
_cell_length_b                   15.5705(16)
_cell_length_c                   17.2632(17)
_cell_measurement_reflns_used    789
_cell_measurement_temperature    140.0(3)
_cell_measurement_theta_max      20.4520
_cell_measurement_theta_min      3.4770
_cell_volume                     2313.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007; Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -48.00   49.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0347   77.0000 -150.0000 97

  2 omega  -40.00   49.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0347   57.0000  -30.0000 89

  3 omega  -25.00    9.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0347  -99.0000    0.0000 34

  4 omega  -85.00   10.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0347  -77.0000   90.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.3709
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14047
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.220
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method 'slow crystallisation of crude oil'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.3359
_refine_ls_R_factor_gt           0.0982
_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^)+(0.0032P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2532
_reflns_number_total             9352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra07007h2.cif
_cod_data_source_block           BArF11Cl5
_cod_database_code               7225036
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C16A(H16A), C18A(H18A), C14B(H14B), C16B(H16B), C18B(H18B)
;
_shelx_res_checksum              51176
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'