Adducts of Donor-Functionalized Ar3P with the Soft Lewis Acid I2: Probing Simultaneous Lewis Acidity and Basicity at Internally Solvated P(III) Centers.
Borys, Andryj M.; Clark, Ewan R.; Inorganic chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00278

data_4345967
_publ_section_title
;
 Adducts of Donor-Functionalized Ar3P with the Soft Lewis Acid I2: Probing
 Simultaneous Lewis Acidity and Basicity at Internally Solvated P(III)
 Centers.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00278
_journal_year                    2017
_chemical_formula_moiety         'C20 H20 I N P, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C53 H34 B Cl2 F24 I N P'
_chemical_formula_weight         1380.39
_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
_audit_creation_date             2017-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90.5505(10)
_cell_angle_beta                 92.5441(9)
_cell_angle_gamma                109.5891(12)
_cell_formula_units_Z            2
_cell_length_a                   12.50066(15)
_cell_length_b                   13.24451(17)
_cell_length_c                   17.59462(19)
_cell_measurement_reflns_used    80740
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4230
_cell_measurement_theta_min      3.5160
_cell_volume                     2740.82(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -82.00  39.00   1.00    2.00    --  -41.14  19.00   0.00  121
  2  \w     23.00  97.00   1.00    2.00    --   41.14-125.00   0.00   74
  3  \w     13.00 113.00   1.00    2.00    --   41.14  57.00-120.00  100
  4  \w      9.00 117.00   1.00    2.00    --   41.14  77.00  30.00  108
  5  \w     13.00 113.00   1.00    2.00    --   41.14  57.00-180.00  100
  6  \w    -31.00  69.00   1.00    2.00    --   41.14 -57.00 150.00  100
  7  \w      9.00 117.00   1.00    2.00    --   41.14  77.00 -60.00  108
  8  \w     17.00 115.00   1.00    2.00    --   41.14  38.00  60.00   98
  9  \w      9.00 117.00   1.00    2.00    --   41.14  77.00-180.00  108
 10  \w      5.00  34.00   1.00    2.00    --   41.14  87.00-144.09   29
 11  \w      9.00 117.00   1.00    2.00    --   41.14  77.00 -90.00  108
 12  \w      1.00  82.00   1.00    2.00    --   41.14 -99.00  60.00   81
 13  \w      9.00 117.00   1.00    2.00    --   41.14  77.00  90.00  108
 14  \w      1.00  82.00   1.00    2.00    --   41.14 -99.00  90.00   81
 15  \w     79.00 178.00   1.00    5.00    --  112.00  77.00 -60.00   99
 16  \w     83.00 178.00   1.00    5.00    --  112.00  61.00  90.00   95
 17  \w     36.00 116.00   1.00    5.00    --  112.00-111.00-150.00   80
 18  \w     79.00 178.00   1.00    5.00    --  112.00  77.00  60.00   99
 19  \w     39.00 138.00   1.00    5.00    --  112.00 -45.00 120.00   99
 20  \w     79.00 178.00   1.00    5.00    --  112.00  77.00  90.00   99
 21  \w     36.00 116.00   1.00    5.00    --  112.00-111.00   0.00   80
 22  \w     79.00 178.00   1.00    5.00    --  112.00  77.00-120.00   99
 23  \w     79.00 178.00   1.00    5.00    --  112.00  77.00  30.00   99
 24  \w     79.00 178.00   1.00    5.00    --  112.00  77.00-150.00   99
 25  \w     79.00 178.00   1.00    5.00    --  112.00  77.00 120.00   99
 26  \w     83.00 178.00   1.00    5.00    --  112.00  61.00-120.00   95
 27  \w     79.00 178.00   1.00    5.00    --  112.00  77.00 -90.00   99
 28  \w     83.00 178.00   1.00    5.00    --  112.00  61.00-150.00   95
 29  \w     83.00 178.00   1.00    5.00    --  112.00  61.00   0.00   95
 30  \w     83.00 178.00   1.00    5.00    --  112.00  61.00 150.00   95
 31  \w     83.00 178.00   1.00    5.00    --  112.00  61.00  30.00   95
 32  \w     36.00 116.00   1.00    5.00    --  112.00-111.00 -60.00   80
 33  \w     83.00 178.00   1.00    5.00    --  112.00  61.00 120.00   95
 34  \w     83.00 178.00   1.00    5.00    --  112.00  61.00 -90.00   95
 35  \w     36.00 145.00   1.00    5.00    --  112.00 -77.00-180.00  109
 36  \w     83.00 178.00   1.00    5.00    --  112.00  61.00 -60.00   95
 37  \w     29.00 109.00   1.00    5.00    --  112.00 -94.00 120.00   80
 38  \w     79.00 178.00   1.00    5.00    --  112.00  77.00 150.00   99
 39  \w     36.00 116.00   1.00    5.00    --  112.00-111.00  90.00   80
 40  \w     83.00 178.00   1.00    5.00    --  112.00  61.00-180.00   95
 41  \w     86.00 178.00   1.00    5.00    --  112.00  45.00 -90.00   92
 42  \w     79.00 178.00   1.00    5.00    --  112.00  77.00 -30.00   99
 43  \w     29.00 109.00   1.00    5.00    --  112.00 -94.00  30.00   80
 44  \w     83.00 178.00   1.00    5.00    --  112.00  61.00  60.00   95
 45  \w     83.00 178.00   1.00    5.00    --  112.00  61.00 -30.00   95
 46  \w     79.00 178.00   1.00    5.00    --  112.00  77.00   0.00   99
 47  \w     79.00 178.00   1.00    5.00    --  112.00  77.00-180.00   99
 48  \w     29.00 109.00   1.00    5.00    --  112.00 -94.00 150.00   80
 49  \w   -115.00 -17.00   1.00    2.00    --  -41.14 -38.00  90.00   98
 50  \w     23.00  97.00   1.00    2.00    --   41.14-125.00-120.00   74
 51  \w     11.00 114.00   1.00    2.00    --   41.14  68.00-165.97  103
 52  \w     13.00 113.00   1.00    2.00    --   41.14  57.00  60.00  100
 53  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00-150.00  176
 54  \w     13.00 113.00   1.00    2.00    --   41.14  57.00 -30.00  100
 55  \w     13.00 113.00   1.00    2.00    --   41.14  57.00 -90.00  100
 56  \w      9.00 117.00   1.00    2.00    --   41.14  77.00  60.00  108
 57  \w      0.00 121.00   1.00    2.00    --   41.14  19.00-150.00  121
 58  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00-180.00  176
 59  \w     17.00 115.00   1.00    2.00    --   41.14  38.00  90.00   98
 60  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00-120.00  176
 61  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00 -90.00  176
 62  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00 -60.00  176
 63  \w    -47.00 129.00   1.00    2.00    --   41.14   0.00 -30.00  176
 64  \w     17.00 115.00   1.00    2.00    --   41.14  38.00-120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0673951000
_diffrn_orient_matrix_UB_12      0.0441326000
_diffrn_orient_matrix_UB_13      0.0755386000
_diffrn_orient_matrix_UB_21      -0.1085910000
_diffrn_orient_matrix_UB_22      -0.0500839000
_diffrn_orient_matrix_UB_23      0.0437262000
_diffrn_orient_matrix_UB_31      0.0286501000
_diffrn_orient_matrix_UB_32      -0.1039101000
_diffrn_orient_matrix_UB_33      0.0082954000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            96039
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.851
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         9767
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0447P)^2^+4.2926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9710
_reflns_number_total             9767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           '[3b]BArF'
_cod_database_code               4345967
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C53 H34 B Cl2 F24 I1 N1 P1'
_chemical_oxdiff_usercomment     'ABS-144 NMe2 BArF Salt'
_cell_oxdiff_angle_alpha         90.5505(10)
_cell_oxdiff_angle_beta          92.5441(9)
_cell_oxdiff_angle_gamma         109.5891(12)
_cell_oxdiff_length_a            12.50066(15)
_cell_oxdiff_length_b            13.24451(17)
_cell_oxdiff_length_c            17.59462(19)
_cell_oxdiff_measurement_reflns_used 80740
_cell_oxdiff_volume              2740.82(6)
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
 F5-C020 \\sim F2-C020 \\sim F4-C020 \\sim F1-C020 \\sim F6-C020 \\sim F3-C020
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.02
 F9-C021 \\sim F11-C021 \\sim F8-C021 \\sim F10-C021 \\sim F7-C021 \\sim
F12-C021
 with sigma of 0.02
 F13-F14 \\sim F14-F15 \\sim F15-F13
 with sigma of 0.02
 F15-C01J \\sim F13-C01J \\sim F14-C01J
 with sigma of 0.02
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F22-F23 \\sim F23-F24 \\sim F24-F22
 with sigma of 0.02
 F23-C01S \\sim F20-C01S \\sim F21-C01S \\sim F24-C01S \\sim F19-C01S \\sim
F22-C01S
 with sigma of 0.02
 F28-F29 \\sim F29-F30 \\sim F30-F28
 with sigma of 0.02
 F29-C01R \\sim F28-C01R \\sim F30-C01R
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5) = Uanis(F1)
Uanis(F6) = Uanis(F2)
Uanis(F4) = Uanis(F3)
Uanis(F7) = Uanis(F11)
Uanis(F9) = Uanis(F10)
Uanis(F23) = Uanis(F19)
Uanis(F24) = Uanis(F20)
Uanis(F21) = Uanis(F22)
Uanis(F12) = Uanis(F8)
4. Others
 Sof(F5)=Sof(F6)=Sof(F4)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(2)
 Sof(F10)=Sof(F12)=Sof(F11)=FVAR(2)
 Sof(F22)=Sof(F24)=Sof(F23)=1-FVAR(3)
 Sof(F20)=Sof(F21)=Sof(F19)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C02B(H02H,H02I)
5.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C013(H013), C014(H014), C017(H017), C01D(H01D), C01F(H01F),
 C01G(H01G), C01I(H01I), C01L(H01L), C01M(H01M), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Z(H01Z), C023(H023), C024(H024), C026(H026), C028(H028),
 C029(H029), C02A(H02G)
5.c Idealised Me refined as rotating group:
 C025(H02A,H02B,H02C), C027(H02D,H02E,H02F)
;
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.727