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_4345963
_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 H19 I2 O2 P'
_chemical_formula_sum            'C20 H19 I2 O2 P'
_chemical_formula_weight         576.12
_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
_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                90.3592(17)
_cell_angle_beta                 94.2694(18)
_cell_angle_gamma                95.4542(16)
_cell_formula_units_Z            2
_cell_length_a                   8.76192(19)
_cell_length_b                   10.48116(19)
_cell_length_c                   11.4220(3)
_cell_measurement_reflns_used    27595
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.2830
_cell_measurement_theta_min      2.5960
_cell_volume                     1041.20(4)
_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    -17.00  83.00   1.00    1.00    --   11.23  57.00-180.00  100
  2  \w    -17.00  83.00   1.00    1.00    --   11.23  57.00 -30.00  100
  3  \w    -61.00  39.00   1.00    1.00    --   11.23 -57.00  30.00  100
  4  \w    -17.00  83.00   1.00    1.00    --   11.23  57.00  60.00  100
  5  \w     35.00 100.00   1.00    1.00    --   11.23 178.00  60.00   65
  6  \w    -20.00  52.00   1.00    1.00    --   11.23 -99.00 150.00   72
  7  \w    -13.00  86.00   1.00    1.00    --   11.23  38.00 120.00   99
  8  \w    -11.00  58.00   1.00    1.00    --   11.23-110.00-103.00   69
  9  \w    -68.00 -23.00   1.00    1.00    --  -11.77 125.00 -86.91   45
 10  \w    -20.00  52.00   1.00    1.00    --   11.23 -99.00-180.00   72
 11  \w     34.00  98.00   1.00    1.00    --   11.23-178.00-150.00   64
 12  \w    -57.00  -8.00   1.00    1.00    --  -11.77 106.00 124.27   49
 13  \w    -54.00  -4.00   1.00    1.00    --  -11.77 101.00-119.80   50
 14  \w    -85.00 -37.00   1.00    1.00    --  -11.77 151.00  -5.43   48
 15  \w    -20.00  29.00   1.00    1.00    --  -11.77 -99.00-180.00   49
 16  \w    -88.00 -39.00   1.00    1.00    --  -11.77 155.00  42.28   49
 17  \w    -77.00  99.00   1.00    1.00    --   11.23   0.00-180.00  176
 18  \w    -77.00  99.00   1.00    1.00    --   11.23   0.00-150.00  176
 19  \w    -77.00   2.00   1.00    1.00    --   11.23   0.00-120.00   79
 20  \w    -80.00 -34.00   1.00    1.00    --  -11.77 144.00 -79.95   46
;
_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      -0.0666901000
_diffrn_orient_matrix_UB_12      -0.0261322000
_diffrn_orient_matrix_UB_13      -0.0341748000
_diffrn_orient_matrix_UB_21      -0.0276700000
_diffrn_orient_matrix_UB_22      -0.0309972000
_diffrn_orient_matrix_UB_23      0.0503435000
_diffrn_orient_matrix_UB_31      -0.0379166000
_diffrn_orient_matrix_UB_32      0.0545767000
_diffrn_orient_matrix_UB_33      0.0132723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42519
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.493
_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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0152P)^2^+1.3003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4098
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           2d
_cod_database_code               4345963
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 P1 O2 I2 H19'
_chemical_oxdiff_usercomment     'ABS-104 Rerun Bis-methoxy'
_cell_oxdiff_angle_alpha         90.3592(17)
_cell_oxdiff_angle_beta          94.2694(18)
_cell_oxdiff_angle_gamma         95.4542(16)
_cell_oxdiff_length_a            8.76192(19)
_cell_oxdiff_length_b            10.48116(19)
_cell_oxdiff_length_c            11.4220(3)
_cell_oxdiff_measurement_reflns_used 27595
_cell_oxdiff_volume              1041.20(4)
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00A(H00A), C00C(H00C), C00D(H00D),
 C00G(H00G), C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M), C00O(H00O),
 C00P(H00P)
2.b Idealised Me refined as rotating group:
 C00K(H00B,H00E,H00F), C00N(H00H,H00K,H00N)
;
_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.703