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_1548379
_publ_section_title
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 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 H9.58 N, C13 H9.42 N, 2(C7 H8)'
_chemical_formula_sum            'C72 H47 B F24 N2'
_chemical_formula_weight         1406.93
_chemical_name_systematic
;
 ? 
;
_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             2017-05-23
_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                 133.202(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.307(4)
_cell_length_b                   18.043(3)
_cell_length_c                   19.611(4)
_cell_measurement_reflns_used    3448
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.30
_cell_volume                     6270(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19268
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1072 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.8700.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7703
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+9.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                4924
_reflns_number_total             7703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp7b09285_si_003.cif
_cod_data_source_block           a
_cod_original_cell_volume        6269.3(19)
_cod_database_code               1548379
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All F(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1S-C2S
 1.51 with sigma of 0.02
 N2-H2
 0.85 with sigma of 0.02
 N1-H1
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7S \\sim C2S \\sim C6S \\sim C3S \\sim C1S \\sim C5S \\sim C4S: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C5S' \\sim C1S' \\sim C2S' \\sim C7S' \\sim C3S' \\sim C6S' \\sim C4S': within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C7S)=Sof(H7S)=Sof(C2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=
 Sof(H5S)=Sof(C6S)=Sof(H6S)=Sof(C1S)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=1-FVAR(1)
 Sof(H1)=0.5*(1-FVAR(2))
 Sof(H2)=0.5*FVAR(2)
 Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C6S')=Sof(H6S')=Sof(C7S')=
 Sof(H7S')=Sof(C2S')=Sof(C3S')=Sof(H3S')=Sof(C4S')=Sof(H4S')=Sof(C5S')=
 Sof(H5S')=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C22(H22), C16(H16), C29(H29), C10(H10), C19(H19), C4(H4),
 C14(H14), C3(H3), C7(H7), C11(H11), C12(H12), C13(H13), C5(H5), C6(H6),
 C6S'(H6S'), C7S'(H7S'), C3S'(H3S'), C4S'(H4S'), C5S'(H5S'), C7S(H7S), C3S(H3S),
  C4S(H4S), C5S(H5S), C6S(H6S)
5.b Fitted hexagon refined as free rotating group:
 C6S'(C7S',C2S',C3S',C4S',C5S'), C7S(C2S,C3S,C4S,C5S,C6S)
5.c Idealised Me refined as rotating group:
 C1S'(H1SA,H1SB,H1SC), C1S(H1SD,H1SE,H1SF)
;
_olex2_submission_special_instructions 'No special instructions were received'