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_4345964
_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         'C22 H25 I N2 P, I'
_chemical_formula_sum            'C22 H25 I2 N2 P'
_chemical_formula_weight         602.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5752(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.94007(14)
_cell_length_b                   42.9758(6)
_cell_length_c                   12.85504(19)
_cell_measurement_reflns_used    26398
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2970
_cell_measurement_theta_min      2.4390
_cell_volume                     4681.70(13)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5775
_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    -13.00  86.00   0.30    8.00    --   11.38  38.00   0.00  330
  2  \w    -18.20  52.00   0.30    8.00    --   11.38 -99.00  60.00  234
  3  \w    -17.00  78.10   0.30    8.00    --   11.38  57.00  90.00  317
  4  \w     35.00  77.00   0.30    8.00    --   11.38 178.00 -60.00  140
  5  \w     36.00  95.10   0.30    8.00    --   11.38 178.00-150.00  197
  6  \w    -16.00  87.20   0.30    8.00    --   11.38  77.00-150.00  344
  7  \w    -61.00  39.50   0.30    8.00    --   11.38 -57.00 -60.00  335
  8  \w    -69.00 -34.20   0.30    8.00    --  -12.01 126.00-159.79  116
  9  \w    -81.00 -54.00   0.30    8.00    --  -12.01 145.00  74.61   90
;
_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      -0.0490334000
_diffrn_orient_matrix_UB_12      0.0124923000
_diffrn_orient_matrix_UB_13      0.0051373000
_diffrn_orient_matrix_UB_21      -0.0190963000
_diffrn_orient_matrix_UB_22      0.0031218000
_diffrn_orient_matrix_UB_23      -0.0569277000
_diffrn_orient_matrix_UB_31      -0.0650840000
_diffrn_orient_matrix_UB_32      -0.0103252000
_diffrn_orient_matrix_UB_33      -0.0109960000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            74293
_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         26.372
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.838
_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    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+5.5423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8282
_reflns_number_total             9569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           2e
_cod_database_code               4345964
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44 H50 N4 P2 I4'
_reflns_odcompleteness_completeness 99.93
_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:
 C22(H22), C10(H10), C41(H41), C19(H19), C18(H18), C42(H42), C11(H11),
 C21(H21), C12(H12), C35(H35), C2(H2), C43(H43), C24(H24), C44(H44), C13(H13),
 C20(H20), C40(H40), C5(H5), C33(H33), C3(H3), C32(H32), C34(H34), C4(H4),
 C27(H27), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              5099
_shelx_hkl_checksum              54825
_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 1.133
_oxdiff_exptl_absorpt_empirical_full_min 0.880