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_4345969
_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 I O2 P, I3, C H2 Cl2'
_chemical_formula_sum            'C21 H21 Cl2 I4 O2 P'
_chemical_formula_weight         914.85
_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                 103.2846(17)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   14.5165(2)
_cell_length_b                   17.6860(3)
_cell_length_c                   22.1653(4)
_cell_measurement_reflns_used    46077
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5650
_cell_measurement_theta_min      2.6830
_cell_volume                     5538.41(16)
_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    -22.00  87.00   1.00   42.50    --   10.88  77.00-150.00  109
  2  \w    -83.00  17.00   1.00   42.50    --  -11.35 -57.00 -60.00  100
  3  \w    -20.00  30.00   1.00   42.50    --  -11.35 -99.00 -60.00   50
  4  \w    -39.00  62.00   1.00   42.50    --  -11.35  57.00  90.00  101
  5  \w     34.00  98.00   1.00   42.50    --   10.88-178.00  60.00   64
  6  \w     11.00  46.00   1.00   42.50    --   10.88-142.00   2.00   35
  7  \w    -20.00  52.00   1.00   42.50    --   10.88 -99.00-120.00   72
  8  \w      4.00  69.00   1.00   42.50    --   10.88-128.00 173.00   65
  9  \w    -86.00  13.00   1.00   42.50    --  -11.35 -38.00  30.00   99
 10  \w    -39.00  62.00   1.00   42.50    --  -11.35  57.00   0.00  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      0.0176653000
_diffrn_orient_matrix_UB_12      -0.0196532000
_diffrn_orient_matrix_UB_13      0.0281706000
_diffrn_orient_matrix_UB_21      -0.0023132000
_diffrn_orient_matrix_UB_22      0.0337841000
_diffrn_orient_matrix_UB_23      0.0168493000
_diffrn_orient_matrix_UB_31      -0.0469433000
_diffrn_orient_matrix_UB_32      -0.0090490000
_diffrn_orient_matrix_UB_33      0.0016641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            109911
_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         26.369
_diffrn_reflns_theta_min         2.212
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.746
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.442
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.799
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         11327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0349P)^2^+32.7033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10156
_reflns_number_total             11327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00278_si_002.cif
_cod_data_source_block           '[3d]I3'
_cod_original_cell_volume        5538.43(16)
_cod_database_code               4345969
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'P1 I4 C21 O1 Cl2 H19'
_chemical_oxdiff_usercomment     'ABS-164 bis-methoxy triiodide salt'
_cell_oxdiff_angle_alpha         90.0275(14)
_cell_oxdiff_angle_beta          103.3298(14)
_cell_oxdiff_angle_gamma         89.9780(14)
_cell_oxdiff_length_a            14.5177(2)
_cell_oxdiff_length_b            17.6793(3)
_cell_oxdiff_length_c            22.1761(4)
_cell_oxdiff_measurement_reflns_used 46068
_cell_oxdiff_volume              5538.43(17)
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C01N(H01X,H01Y), C01O(H01Z,H)
2.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C014(H014),
 C015(H015), C016(H016), C017(H017), C01A(H01D), C01B(H01P), C01C(H01Q),
 C01D(H01R), C01E(H01E), C01F(H01F), C01G(H01S), C01H(H01H), C01I(H01T),
 C01J(H01J), C01K(H01K)
2.c Idealised Me refined as rotating group:
 C018(H01A,H01B,H01C), C019(H01M,H01N,H01O), C01L(H01U,H01V,H01W), C01M(H01G,
 H01I,H01L)
;
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.632