Self-association of diphenylpnictoginic acids in solution and solid state: covalent vs hydrogen bonding
Yakubenko, Artyom A.; Puzyk, Aleksandra M.; Korostelev, Vladislav O.; Mulloyarova, Valeriia V.; Tupikina, Elena Yu.; Tolstoy, Peter; Antonov, Alexander S.; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D2CP00286H

data_7244598
_publ_section_title
;
 Self-association of diphenylpnictoginic acids in solution and solid
 state: covalent vs hydrogen bonding
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D2CP00286H
_journal_year                    2022
_chemical_formula_moiety         'C18 H15 Cl2 Sb'
_chemical_formula_sum            'C18 H15 Cl2 Sb'
_chemical_formula_weight         423.95
_chemical_name_systematic        'Triphenylantimony dichloride'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.12210(10)
_cell_length_b                   9.41070(10)
_cell_length_c                   15.8718(2)
_cell_measurement_reflns_used    14422
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      76.5660
_cell_measurement_theta_min      5.6010
_cell_volume                     1654.46(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -63.00 -22.00   0.50    0.40    --  -47.44 101.00 147.00   82
  2  \w    -17.00  79.00   0.50    0.40    --   47.44-101.00  43.00  192
  3  \w   -171.00 -88.00   0.50    1.60    -- -106.00-101.00  43.00  166
  4  \w   -104.00 -66.00   0.50    1.60    -- -106.00 101.00 147.00   76
  5  \w     41.00  83.00   0.50    1.60    --  106.50-101.00  43.00   84
  6  \w    119.00 144.00   0.50    1.60    --  106.50 101.00 147.00   50
  7  \w   -114.00 -75.00   0.50    0.40    --  -47.44-125.00-180.00   78
  8  \w    -42.00  21.00   0.50    0.40    --  -47.44  37.00 -90.00  126
  9  \w     80.00 118.00   0.50    0.40    --   47.44 125.00 -30.00   76
 10  \w     75.00 102.00   0.50    0.40    --   47.44 125.00 -90.00   54
 11  \w    -71.00 -36.00   0.50    1.60    -- -106.00  61.00 -90.00   70
 12  \w   -172.00 -93.00   0.50    1.60    -- -106.00 -45.00  90.00  158
 13  \w    -71.00 -33.00   0.50    1.60    -- -106.00  61.00   0.00   76
 14  \w   -142.00 -76.00   0.50    1.60    -- -106.00-125.00-150.00  132
 15  \w    -70.00 -36.00   0.50    1.60    -- -106.00  61.00 -30.00   68
 16  \w    -62.00 -36.00   0.50    1.60    -- -106.00  61.00 150.00   52
 17  \w    -71.00 -33.00   0.50    1.60    -- -106.00  61.00 -60.00   76
 18  \w     45.00  70.00   0.50    1.60    --  106.50-125.00   0.00   50
 19  \w     45.00  94.00   0.50    1.60    --  106.50 -77.00  60.00   98
 20  \w     40.00  97.00   0.50    1.60    --  106.50 -94.00  60.00  114
 21  \w     37.00  69.00   0.50    1.60    --  106.50 -61.00  90.00   64
 22  \w     34.00  59.00   0.50    1.60    --  106.50 -61.00-180.00   50
 23  \w     76.00 102.00   0.50    1.60    --  106.50-101.00  43.00   52
 24  \w      2.00  28.00   0.50    0.40    --  -47.44  19.00-150.00   52
 25  \w    -41.00  26.00   0.50    0.40    --  -47.44  37.00-180.00  134
 26  \w    -23.00  22.00   0.50    0.40    --   47.44 -19.00  30.00   90
 27  \w     81.00 107.00   0.50    0.40    --   47.44 125.00 -60.00   52
 28  \w   -176.00-134.00   0.50    1.60    -- -106.00 -45.00 -30.00   84
 29  \w    -64.00 -38.00   0.50    1.60    -- -106.00  61.00 120.00   52
 30  \w    -59.00 -33.00   0.50    1.60    -- -106.00 125.00  90.00   52
 31  \w   -112.00 -78.00   0.50    1.60    -- -106.00 125.00 -60.00   68
 32  \w   -111.00 -69.00   0.50    1.60    -- -106.00 125.00 150.00   84
 33  \w   -131.00-105.00   0.50    1.60    -- -106.00 -61.00 -60.00   52
 34  \w   -129.00 -93.00   0.50    1.60    -- -106.00 -45.00 -30.00   72
 35  \w   -177.00-152.00   0.50    1.60    -- -106.00 -30.00-150.00   50
 36  \w   -143.00 -96.00   0.50    1.60    -- -106.00 -30.00-150.00   94
 37  \w   -175.00-150.00   0.50    1.60    -- -106.00 -61.00 -60.00   50
 38  \w   -108.00 -83.00   0.50    1.60    -- -106.00 114.00 -85.31   50
 39  \w     40.00  70.00   0.50    1.60    --  106.50 -61.00  60.00   60
 40  \w    149.00 176.00   0.50    1.60    --  106.50  45.00-150.00   54
 41  \w     69.00 107.00   0.50    1.60    --  106.50-125.00-120.00   76
 42  \w     76.00 107.00   0.50    1.60    --  106.50-106.00 -34.72   62
 43  \w     38.00  64.00   0.50    1.60    --  106.50 -61.00 -30.00   52
 44  \w     34.00  60.00   0.50    1.60    --  106.50 -61.00 120.00   52
 45  \w     42.00  68.00   0.50    1.60    --  106.50-125.00-120.00   52
 46  \w     39.00  64.00   0.50    1.60    --  106.50 -61.00   0.00   50
 47  \w     71.00 103.00   0.50    1.60    --  106.50 -94.00-150.00   64
 48  \w     95.00 178.00   0.50    1.60    --  106.50  30.00-120.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0491272000
_diffrn_orient_matrix_UB_12      -0.0144533000
_diffrn_orient_matrix_UB_13      0.0872482000
_diffrn_orient_matrix_UB_21      -0.0434103000
_diffrn_orient_matrix_UB_22      0.1555851000
_diffrn_orient_matrix_UB_23      -0.0055756000
_diffrn_orient_matrix_UB_31      -0.1226447000
_diffrn_orient_matrix_UB_32      -0.0492041000
_diffrn_orient_matrix_UB_33      -0.0429400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19558
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.492
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_min         3.991
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.634
_refine_diff_density_min         -1.795
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0389P)^2^+9.1087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2798
_reflns_number_total             2985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp00286h3.cif
_cod_data_source_block           0ver0-19209_art-038
_cod_database_code               7244598
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H17 Sb1 O2'
_shelx_estimated_absorpt_t_max   0.565
_shelx_estimated_absorpt_t_min   0.359
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C12(H12), C2(H2), C11(H11), C8(H8), C14(H14), C10(H10),
 C17(H17), C3(H3), C18(H18), C4(H4), C15(H15), C16(H16), C9(H9)
;
_shelx_res_checksum              99456
_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 1.538
_oxdiff_exptl_absorpt_empirical_full_min 0.624