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_4345966
_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
'C19 H17 I O P, C32 H12 B F24, C6 H14, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C57.5 H44 B Cl F24 I O P'
_chemical_formula_weight         1411.05
_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             2017-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                86.9054(14)
_cell_angle_beta                 82.8373(15)
_cell_angle_gamma                71.4746(17)
_cell_formula_units_Z            2
_cell_length_a                   12.3441(3)
_cell_length_b                   13.0277(2)
_cell_length_c                   19.3179(3)
_cell_measurement_reflns_used    55352
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1850
_cell_measurement_theta_min      3.5750
_cell_volume                     2922.31(10)
_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      100.00(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    -47.00 129.00   1.00    5.00    --   41.14   0.00 -90.00  176
  2  \w      9.00 117.00   1.00    5.00    --   41.14  77.00 -30.00  108
  3  \w     23.00  97.00   1.00    5.00    --   41.14-125.00  30.00   74
  4  \w     13.00 113.00   1.00    5.00    --   41.14  57.00 150.00  100
  5  \w     17.00 115.00   1.00    5.00    --   41.14  38.00 -60.00   98
  6  \w      1.00  82.00   1.00    5.00    --   41.14 -99.00 -60.00   81
  7  \w    -31.00  69.00   1.00    5.00    --   41.14 -57.00 150.00  100
  8  \w      9.00 117.00   1.00    5.00    --   41.14  77.00-180.00  108
  9  \w      9.00 117.00   1.00    5.00    --   41.14  77.00  90.00  108
 10  \w      9.00 117.00   1.00    5.00    --   41.14  77.00   0.00  108
 11  \w     23.00  97.00   1.00    5.00    --   41.14-125.00 120.00   74
 12  \w      9.00 117.00   1.00    5.00    --   41.14  77.00-120.00  108
 13  \w     17.00 115.00   1.00    5.00    --   41.14  38.00  90.00   98
 14  \w     36.00 116.00   1.00   20.00    --  112.00-111.00  90.00   80
 15  \w     39.00 138.00   1.00   20.00    --  112.00 -45.00  90.00   99
 16  \w     79.00 178.00   1.00   20.00    --  112.00  77.00  30.00   99
 17  \w     29.00 109.00   1.00   20.00    --  112.00 -94.00-120.00   80
 18  \w     40.00 141.00   1.00   20.00    --  112.00 -61.00-150.00  101
 19  \w     79.00 178.00   1.00   20.00    --  112.00  77.00-150.00   99
 20  \w     79.00 178.00   1.00   20.00    --  112.00  77.00 -30.00   99
 21  \w     79.00 178.00   1.00   20.00    --  112.00  77.00  90.00   99
 22  \w    101.00 178.00   1.00   20.00    --  112.00 112.00 159.00   77
 23  \w     79.00 178.00   1.00   20.00    --  112.00  77.00 150.00   99
 24  \w     83.00 178.00   1.00   20.00    --  112.00  61.00  30.00   95
 25  \w     83.00 178.00   1.00   20.00    --  112.00  61.00-180.00   95
 26  \w     36.00 145.00   1.00   20.00    --  112.00 -77.00  90.00  109
 27  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 120.00   95
 28  \w     79.00 178.00   1.00   20.00    --  112.00  77.00 120.00   99
 29  \w     79.00 178.00   1.00   20.00    --  112.00  77.00 -60.00   99
 30  \w     79.00 178.00   1.00   20.00    --  112.00  77.00 -90.00   99
 31  \w     83.00 178.00   1.00   20.00    --  112.00  61.00  60.00   95
 32  \w     29.00 109.00   1.00   20.00    --  112.00 -94.00   0.00   80
 33  \w     83.00 178.00   1.00   20.00    --  112.00  61.00-150.00   95
 34  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 -90.00   95
 35  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 -30.00   95
 36  \w     79.00 178.00   1.00   20.00    --  112.00  77.00   0.00   99
 37  \w     83.00 178.00   1.00   20.00    --  112.00  61.00  90.00   95
 38  \w     79.00 178.00   1.00   20.00    --  112.00  77.00-180.00   99
 39  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 150.00   95
 40  \w     86.00 178.00   1.00   20.00    --  112.00  45.00  30.00   92
 41  \w     86.00 178.00   1.00   20.00    --  112.00  45.00  90.00   92
 42  \w     83.00 178.00   1.00   20.00    --  112.00  61.00 -60.00   95
 43  \w     79.00 178.00   1.00   20.00    --  112.00  77.00  60.00   99
 44  \w     79.00 178.00   1.00   20.00    --  112.00  77.00-120.00   99
 45  \w     83.00 178.00   1.00   20.00    --  112.00  61.00-120.00   95
 46  \w     36.00 116.00   1.00   20.00    --  112.00-111.00-150.00   80
 47  \w     83.00 178.00   1.00   20.00    --  112.00  61.00   0.00   95
 48  \w     36.00 116.00   1.00   20.00    --  112.00-111.00 -30.00   80
 49  \w   -115.00 -17.00   1.00    5.00    --  -41.14 -38.00 -90.00   98
 50  \w     17.00 115.00   1.00    5.00    --   41.14  38.00-180.00   98
 51  \w     17.00 115.00   1.00    5.00    --   41.14  38.00  60.00   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      0.0842769000
_diffrn_orient_matrix_UB_12      0.0444630000
_diffrn_orient_matrix_UB_13      0.0317145000
_diffrn_orient_matrix_UB_21      0.0325632000
_diffrn_orient_matrix_UB_22      0.0452188000
_diffrn_orient_matrix_UB_23      -0.0721494000
_diffrn_orient_matrix_UB_31      -0.0968907000
_diffrn_orient_matrix_UB_32      0.1074049000
_diffrn_orient_matrix_UB_33      0.0158210000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0274
_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       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77608
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.031
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_correction_T_min  0.143
_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    1.604
_exptl_crystal_description       plank
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.727
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         10690
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+10.1944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10593
_reflns_number_total             10690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           '[3a]BArF'
_cod_original_cell_volume        2922.31(9)
_cod_original_formula_sum        'C57.50 H44 B Cl F24 I O P'
_cod_database_code               4345966
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C57.5 I1 B1 P1 O1 F24 H44 Cl1'
_chemical_oxdiff_usercomment     'ABS-143 OMe BArF Salt'
_cell_oxdiff_angle_alpha         86.9054(14)
_cell_oxdiff_angle_beta          82.8373(15)
_cell_oxdiff_angle_gamma         71.4746(17)
_cell_oxdiff_length_a            12.3441(3)
_cell_oxdiff_length_b            13.0277(2)
_cell_oxdiff_length_c            19.3179(3)
_cell_oxdiff_measurement_reflns_used 55352
_cell_oxdiff_volume              2922.31(9)
_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
 Cl1-C3 \\sim Cl2-C3
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F4-F5 \\sim F5-F6 \\sim F6-F4
 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-C01X \\sim F10-C01X \\sim F7-C01X \\sim F11-C01X \\sim F8-C01X \\sim
F12-C01X \\sim F1-C01R \\sim F6-
 C01R \\sim F2-C01R \\sim F5-C01R \\sim F3-C01R \\sim F4-C01R
 with sigma of 0.02
 F18-C01V \\sim F14-C01V \\sim F16-C01V \\sim F15-C01V \\sim F17-C01V \\sim
F13-C01V
 with sigma of 0.02
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F16-F17 \\sim F17-F18 \\sim F18-F16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(C3) = Uanis(Cl2)
Uanis(F8) = Uanis(F10)
Uanis(F12) = Uanis(F7)
Uanis(F11) = Uanis(F9)
Uanis(F6) = Uanis(F3)
Uanis(F5) = Uanis(F2)
Uanis(F1) = Uanis(F4)
Uanis(F18) = Uanis(F15)
Uanis(F13) = Uanis(F16)
Uanis(F14) = Uanis(F17)
4. Others
 Sof(F2)=Sof(F3)=Sof(F1)=1-FVAR(1)
 Sof(F6)=Sof(F4)=Sof(F5)=FVAR(1)
 Sof(F12)=Sof(F10)=Sof(F11)=1-FVAR(2)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(2)
 Sof(F15)=Sof(F14)=Sof(F13)=1-FVAR(3)
 Sof(F18)=Sof(F17)=Sof(F16)=FVAR(3)
 Fixed Sof: Cl1(0.5) Cl2(0.5) C3(0.5) H3A(0.5) H3B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C02A(H02G,H02H), C02B(H02I,H02J), C02C(H02K,H02L), C02E(H02M,H02N), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00Z(H00Z), C010(H010), C011(H011), C014(H014), C016(H016), C017(H017),
 C01N(H01N), C01O(H01O), C01Q(H01Q), C01U(H01U), C01W(H01W), C01Y(H01Y),
 C01Z(H01Z), C021(H021), C022(H022), C023(H023), C024(H024), C025(H025),
 C026(H026), C027(H027)
5.c Idealised Me refined as rotating group:
 C028(H02A,H02B,H02C), C029(H02D,H02E,H02F), C02F(H02O,H02P,H02Q)
;
_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 2.123
_oxdiff_exptl_absorpt_empirical_full_min 0.474