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_4345970
_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, C22 H25 I N2 P'
_chemical_formula_sum            'C22 H25 I4 N2 P'
_chemical_formula_weight         856.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90.0
_cell_angle_beta                 98.650(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.9475(3)
_cell_length_b                   16.4754(4)
_cell_length_c                   13.5533(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3380
_cell_measurement_theta_min      2.8900
_cell_volume                     2637.48(11)
_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 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    -17.00  75.00   1.00  115.00    --   10.88  57.00 -90.00   92
  2  \w    -77.00  12.00   1.00  115.00    --  -11.35 -57.00 -30.00   89
  3  \w    -19.00   9.00   1.00  115.00    --  -11.35 -99.00 -30.00   28
  4  \w    -39.00  62.00   1.00  115.00    --  -11.35  57.00 120.00  101
;
_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      -0.0155466000
_diffrn_orient_matrix_UB_12      -0.0415433000
_diffrn_orient_matrix_UB_13      -0.0019460000
_diffrn_orient_matrix_UB_21      0.0565767000
_diffrn_orient_matrix_UB_22      -0.0107504000
_diffrn_orient_matrix_UB_23      0.0194262000
_diffrn_orient_matrix_UB_31      -0.0131845000
_diffrn_orient_matrix_UB_32      0.0026476000
_diffrn_orient_matrix_UB_33      0.0492057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19253
_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         25.613
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.774
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.687
_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 reddish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0170P)^2^+2.1310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4424
_reflns_number_total             4975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           '[3e]I3'
_cod_original_cell_volume        2637.49(11)
_cod_database_code               4345970
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C22 N2 P1 I4 H25'
_chemical_oxdiff_usercomment     'ABS-165 bis-NMe2 triiodide'
_cell_oxdiff_angle_alpha         90.049(3)
_cell_oxdiff_angle_beta          98.682(3)
_cell_oxdiff_angle_gamma         90.052(4)
_cell_oxdiff_length_a            11.9315(6)
_cell_oxdiff_length_b            16.4979(7)
_cell_oxdiff_length_c            13.5542(4)
_cell_oxdiff_measurement_reflns_used 9986
_cell_oxdiff_volume              2637.49(19)
_reflns_odcompleteness_completeness 99.91
_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:
 C6(H6), C14(H14), C22(H22), C5(H5), C4(H4), C18(H18), C11(H11), C13(H13),
 C20(H20), C12(H12), C19(H19), C3(H3), C21(H21)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_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 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.858
_vrf-plat434_serc051-r1-rf
;
PROBLEM: Short Inter HL..HL Contact I1     ..  I4      ..       3.58 Ang.
RESPONSE: Weak covalent interactions are observed between the phosphorus-bound
iodine atom and the triiodide anion.
;