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_7244607
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   13.01340(10)
_cell_length_b                   23.6265(2)
_cell_length_c                   43.3575(4)
_cell_measurement_reflns_used    25761
_cell_measurement_temperature    100.00(2)
_cell_measurement_theta_max      75.9240
_cell_measurement_theta_min      3.0640
_cell_volume                     13330.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_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    -33.00  -7.00   1.00   12.50    --  -40.38  38.00  90.00   26
  2  \w    -62.00  30.00   1.00   12.50    --  -40.38  38.00-150.00   92
  3  \w      7.00  33.00   1.00   12.50    --   40.38 -99.00 -60.00   26
  4  \w     73.00 109.00   1.00   12.50    --   40.38 178.00  90.00   36
  5  \w    105.00 131.00   1.00   47.50    --  113.00  77.00 -30.00   26
  6  \w    145.00 171.00   1.00   47.50    --  113.00  77.00 -30.00   26
  7  \w    105.00 140.00   1.00   47.50    --  113.00 112.00 150.00   35
  8  \w     45.00  95.00   1.00   47.50    --  113.00-112.00  60.00   50
  9  \w    124.00 173.00   1.00   47.50    --  113.00  77.00  60.00   49
 10  \w    104.00 169.00   1.00   47.50    --  113.00  77.00 -60.00   65
 11  \w     81.00 143.00   1.00   47.50    --  113.00 178.00  90.00   62
 12  \w     58.00  90.00   1.00   12.50    --   40.38-178.00  30.00   32
 13  \w     95.00 129.00   1.00   12.50    --   40.38-178.00  60.00   34
 14  \w    104.00 129.00   1.00   12.50    --   40.38-178.00  30.00   25
 15  \w    109.00 160.00   1.00   47.50    --  113.00  77.00 -90.00   51
 16  \w    123.00 159.00   1.00   47.50    --  113.00 112.00-150.00   36
 17  \w    118.00 162.00   1.00   47.50    --  113.00 112.00-180.00   44
 18  \w     58.00  98.00   1.00   47.50    --  113.00-112.00-120.00   40
 19  \w     41.00 124.00   1.00   47.50    --  113.00 -77.00-150.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0309196000
_diffrn_orient_matrix_UB_12      -0.0579239000
_diffrn_orient_matrix_UB_13      -0.0134680000
_diffrn_orient_matrix_UB_21      -0.0559304000
_diffrn_orient_matrix_UB_22      -0.0146399000
_diffrn_orient_matrix_UB_23      0.0302903000
_diffrn_orient_matrix_UB_31      -0.0996319000
_diffrn_orient_matrix_UB_32      0.0261177000
_diffrn_orient_matrix_UB_33      -0.0128042000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            55699
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.999
_diffrn_reflns_theta_max         65.999
_diffrn_reflns_theta_min         3.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       prism
_exptl_crystal_F_000             6656
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         11598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10667
_reflns_number_total             11598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp00286h3.cif
_cod_data_source_block           0ver0-15669_art-02
_cod_database_code               7244607
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H15 Cl2 Sb1'
_shelx_estimated_absorpt_t_max   0.361
_shelx_estimated_absorpt_t_min   0.213
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C6(H6), C11(H11), C72(H72), C42(H42), C54(H54), C53(H53), C38(H38),
 C51(H51), C18(H18), C40(H40), C21(H21), C41(H41), C5(H5), C12(H12), C39(H39),
 C60(H60), C27(H27), C15(H15), C32(H32), C64(H64), C10(H10), C16(H16), C24(H24),
  C65(H65), C23(H23), C30(H30), C44(H44), C8(H8), C20(H20), C66(H66), C9(H9),
 C62(H62), C48(H48), C35(H35), C14(H14), C3(H3), C68(H68), C71(H71), C63(H63),
 C26(H26), C52(H52), C2(H2), C59(H59), C69(H69), C56(H56), C28(H28), C4(H4),
 C33(H33), C47(H47), C29(H29), C50(H50), C17(H17), C70(H70), C22(H22), C45(H45),
  C58(H58), C57(H57), C34(H34), C46(H46)
;
_shelx_res_checksum              50113
_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 1.497
_oxdiff_exptl_absorpt_empirical_full_min 0.516