NMR Study of Solvation Effect on the Geometry of Proton-Bound Homodimers of Increasing Size.
Gurinov, Andrei A.; Denisov, Gleb S.; Borissova, Alexandra O.; Goloveshkin, Alexander S.; Greindl, Julian; Limbach, Hans-Heinrich; Shenderovich, Ilya G.; The journal of physical chemistry. A 121 (2017) 8697–8705; doi:10.1021/acs.jpca.7b09285

data_1548378
_publ_section_title
;
 NMR Study of Solvation Effect on the Geometry of Proton-Bound Homodimers
 of Increasing Size.
;
_journal_issue                   45
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              8697
_journal_page_last               8705
_journal_paper_doi               10.1021/acs.jpca.7b09285
_journal_volume                  121
_journal_year                    2017
_chemical_formula_moiety
'C32 H12 B F24, C13 H10 N, C13 H9 N, 2(C H Cl3)'
_chemical_formula_sum            'C60 H33 B Cl6 F24 N2'
_chemical_formula_weight         1461.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 124.4790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4747(14)
_cell_length_b                   18.1680(10)
_cell_length_c                   17.2650(18)
_cell_measurement_reflns_used    5667
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.47
_cell_volume                     6069.8(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19909
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0844 before and 0.0345 after correction.
The Ratio of minimum to maximum transmission is 0.8816.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8066
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+22.4746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                5832
_reflns_number_total             8066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp7b09285_si_002.cif
_cod_data_source_block           a
_cod_database_code               1548378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1
 0.85 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1S(H1S)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C27(H27), C19(H19), C16(H16), C3(H3), C7(H7), C4(H4),
 C6(H6), C5(H5), C30(H30), C10(H10), C13(H13), C11(H11), C14(H14), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'