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_4345965
_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         'C18 H15 I2 P'
_chemical_formula_sum            'C18 H15 I2 P'
_chemical_formula_weight         516.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.33101(9)
_cell_length_b                   12.83882(12)
_cell_length_c                   13.61886(13)
_cell_measurement_reflns_used    65164
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0190
_cell_measurement_theta_min      2.5270
_cell_volume                     1806.38(3)
_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)'
_computing_structure_solution    'ShelXT (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    -16.00  85.00   1.00    6.00    --   12.34  57.00  60.00  101
  2  \w     35.00 101.00   1.00    6.00    --   12.34 178.00 -60.00   66
  3  \w    -20.00  88.00   1.00    6.00    --   12.34  77.00-150.00  108
  4  \w    -16.00  85.00   1.00    6.00    --   12.34  57.00  90.00  101
  5  \w    -61.00  40.00   1.00    6.00    --   12.34 -57.00 -60.00  101
  6  \w    -16.00  85.00   1.00    6.00    --   12.34  57.00 -30.00  101
  7  \w    -20.00  53.00   1.00    6.00    --   12.34 -99.00  60.00   73
  8  \w    -37.00  61.00   1.00    6.00    --  -12.80  38.00 150.00   98
  9  \w    -89.00 -39.00   1.00    6.00    --  -12.80 154.00 149.76   50
 10  \w    -88.00 -38.00   1.00    6.00    --  -12.80 153.00  51.09   50
 11  \w    -88.00 -38.00   1.00    6.00    --  -12.80 153.00 -10.05   50
 12  \w    -45.00  63.00   1.00    6.00    --  -12.80  77.00   0.00  108
 13  \w    -89.00 -39.00   1.00    6.00    --  -12.80 154.00-152.11   50
 14  \w    -89.00 -39.00   1.00    6.00    --  -12.80 154.00 -43.86   50
 15  \w    -90.00 -40.00   1.00    6.00    --  -12.80 156.00  99.85   50
 16  \w    -88.00 -38.00   1.00    6.00    --  -12.80 153.00-107.56   50
 17  \w    -37.00  61.00   1.00    6.00    --  -12.80  38.00 -30.00   98
 18  \w    -84.00 -35.00   1.00    6.00    --  -12.80 148.00 -84.28   49
 19  \w    -76.00  61.00   1.00    6.00    --   12.34   0.00-150.00  137
 20  \w    -76.00 100.00   1.00    6.00    --   12.34   0.00-180.00  176
;
_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      0.0001478000
_diffrn_orient_matrix_UB_12      0.0018405000
_diffrn_orient_matrix_UB_13      0.0520421000
_diffrn_orient_matrix_UB_21      0.0002395000
_diffrn_orient_matrix_UB_22      -0.0552289000
_diffrn_orient_matrix_UB_23      0.0017387000
_diffrn_orient_matrix_UB_31      0.0686542000
_diffrn_orient_matrix_UB_32      0.0001920000
_diffrn_orient_matrix_UB_33      -0.0001148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            84204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.079
_diffrn_reflns_theta_min         2.180
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.555
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.101
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             976
_exptl_crystal_preparation
'Addition of one equivalent of iodine to trophenylphosphine in diethyl ether.'
_exptl_crystal_recrystallization_method
'Layering a saturated solution in DCM with diethyl ether.'
_exptl_crystal_size_max          0.785
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 2062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0121P)^2^+1.3979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0369
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4827
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           2g
_cod_database_code               4345965
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H15 P1 I2'
_chemical_oxdiff_usercomment     Ph3PI2
_cell_oxdiff_angle_alpha         89.9941(14)
_cell_oxdiff_angle_beta          90.0035(12)
_cell_oxdiff_angle_gamma         90.0036(11)
_cell_oxdiff_length_a            10.33140(12)
_cell_oxdiff_length_b            12.8357(2)
_cell_oxdiff_length_c            13.6217(2)
_cell_oxdiff_measurement_reflns_used 65164
_cell_oxdiff_volume              1806.38(5)
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C006(H006), C007(H007), C009(H009), C00A(H00A), C00B(H00B),
 C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I),
 C00J(H00J), C00K(H00K), C00L(H00L)
;
_olex2_exptl_crystal_mounting_method MiTeGen.
_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 1.531
_oxdiff_exptl_absorpt_empirical_full_min 0.383