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_4345973
_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         'I3, C20 H19 N P'
_chemical_formula_sum            'C20 H19 I3 N P'
_chemical_formula_weight         685.03
_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
_audit_creation_date             2017-01-23
_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                   18.3990(2)
_cell_length_b                   12.17869(14)
_cell_length_c                   9.99371(12)
_cell_measurement_reflns_used    65309
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2810
_cell_measurement_theta_min      2.6430
_cell_volume                     2239.35(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)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -61.00  38.00   1.00   25.00    --   13.10 -38.00 150.00   99
  2  \w    -61.00  38.00   1.00   25.00    --   13.10 -38.00 -60.00   99
  3  \w    -11.00  87.00   1.00   25.00    --   13.10  38.00 120.00   98
  4  \w    -20.00  54.00   1.00   25.00    --   13.10 -99.00  60.00   74
  5  \w    -11.00  87.00   1.00   25.00    --   13.10  38.00 -30.00   98
  6  \w    -19.00  89.00   1.00   25.00    --   13.10  77.00-150.00  108
  7  \w    -38.00  61.00   1.00   25.00    --  -13.72  38.00-150.00   99
  8  \w    -20.00  27.00   1.00   25.00    --  -13.72 -99.00 -60.00   47
  9  \w    -91.00 -40.00   1.00   25.00    --  -13.72 156.00-177.19   51
 10  \w    -72.00 -26.00   1.00   25.00    --  -13.72 128.00  94.01   46
 11  \w     34.00 100.00   1.00   25.00    --   13.10-178.00-180.00   66
 12  \w    -91.00 -40.00   1.00   25.00    --  -13.72 156.00 136.58   51
 13  \w    -72.00 -26.00   1.00   25.00    --  -13.72 128.00  24.40   46
 14  \w    -90.00 -39.00   1.00   25.00    --  -13.72 155.00 -23.80   51
 15  \w    -20.00  27.00   1.00   25.00    --  -13.72 -99.00  30.00   47
 16  \w    -72.00 -26.00   1.00   25.00    --  -13.72 128.00-111.06   46
 17  \w   -102.00 -57.00   1.00   25.00    --  -13.72-178.00 120.00   45
 18  \w    -89.00 -38.00   1.00   25.00    --  -13.72 153.00 -81.91   51
 19  \w    -75.00  -1.00   1.00   25.00    --   13.10   0.00-120.00   74
 20  \w    -75.00 101.00   1.00   25.00    --   13.10   0.00-150.00  176
 21  \w    -75.00 101.00   1.00   25.00    --   13.10   0.00-180.00  176
 22  \w    -91.00 -40.00   1.00   25.00    --  -13.72 156.00 156.89   51
 23  \w    -89.00 -38.00   1.00   25.00    --  -13.72 153.00  34.37   51
 24  \w    -72.00 -26.00   1.00   25.00    --  -13.72 128.00 134.36   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      -0.0009434000
_diffrn_orient_matrix_UB_12      -0.0134463000
_diffrn_orient_matrix_UB_13      0.0690315000
_diffrn_orient_matrix_UB_21      0.0064153000
_diffrn_orient_matrix_UB_22      -0.0559234000
_diffrn_orient_matrix_UB_23      -0.0158890000
_diffrn_orient_matrix_UB_31      0.0380078000
_diffrn_orient_matrix_UB_32      0.0091013000
_diffrn_orient_matrix_UB_33      0.0044015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            98437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.005
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.253
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.422
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.625
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 1928 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0433P)^2^+3.0483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4534
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           '[4]I3'
_cod_database_code               4345973
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 N1 P1 I3 H19'
_chemical_oxdiff_usercomment     'ABS-201 Thermal rearrangement'
_cell_oxdiff_angle_alpha         90.0058(13)
_cell_oxdiff_angle_beta          90.0049(11)
_cell_oxdiff_angle_gamma         89.9961(11)
_cell_oxdiff_length_a            18.3961(2)
_cell_oxdiff_length_b            12.18036(19)
_cell_oxdiff_length_c            9.99392(15)
_cell_oxdiff_measurement_reflns_used 65309
_cell_oxdiff_volume              2239.35(5)
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C11(H11), C13(H13), C20(H20), C14(H14), C5(H5), C7(H7),
 C4(H4), C6(H6), C16(H16), C19(H19), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.504