Unexpected Solvent Effect on the Binding of Positively-Charged Macrocycles to Neutral Aromatic Hydrocarbons
Wang, Yu-Mei; Yao, Huan; Quan, Mao; Chai, Hongxin; Yang, Liu-Pan; Pan, Ying-Ming; Jiang, Wei; Chemical Communications  (2019) –; doi:10.1039/C9CC06154A

data_7124006
_publ_section_title
;
 Unexpected Solvent Effect on the Binding of Positively-Charged
 Macrocycles to Neutral Aromatic Hydrocarbons
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06154A
_journal_year                    2019
_chemical_formula_moiety         '2(C32 H12 B F24), C72 H74 N4 O8, C Cl2 D2'
_chemical_formula_sum            'C137 H98 B2 Cl2 D2 F48 N4 O8'
_chemical_formula_weight         2936.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-06 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.310(2)
_cell_angle_beta                 84.666(2)
_cell_angle_gamma                67.739(2)
_cell_formula_units_Z            1
_cell_length_a                   13.9528(5)
_cell_length_b                   15.9387(5)
_cell_length_c                   16.2647(6)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100.04
_cell_measurement_theta_max      60.073
_cell_measurement_theta_min      2.808
_cell_volume                     3238.1(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_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_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45782
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        60.207
_diffrn_reflns_theta_max         60.207
_diffrn_reflns_theta_min         2.809
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1198 before and 0.0645 after correction. The Ratio of minimum to maximum transmission is 0.7450. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         9579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+4.5341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8458
_reflns_number_total             9579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06154a2.cif
_cod_data_source_block           p1
_cod_database_code               7124006
_shelx_shelxl_version_number     2014/7
_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. Others
 Fixed Sof: Cl4(0.5) C1(0.5) D1A(0.5) D1B(0.5) Cl0A(0.5)
3.a Ternary CH refined with riding coordinates:
 C025(H025), C02I(H02Q)
3.b Secondary CH2 refined with riding coordinates:
 C022(H02A,H02B), C026(H02C,H02D), C027(H02E,H02F), C029(H02G,H02H), C02B(H02I,
 H02J), C02G(H02N,H02O), C02O(H02W,H02X), C02S(H02,HB), C02T(H0AA,HC), C1(D1A,
 D1B)
3.c Aromatic/amide H refined with riding coordinates:
 C011(H011), C013(H013), C016(H016), C017(H017), C01A(H01A), C01B(H01B),
 C01E(H01E), C01J(H01J), C01K(H01K), C01L(H01L), C01N(H01N), C01O(H01O),
 C01S(H01S), C01V(H01V), C021(H021), C02D(H02K), C02E(H02L), C02F(H02M),
 C02H(H02P), C02J(H02R), C02L(H1AA), C02M(H02S), C02P(H02Y)
3.d Idealised Me refined as rotating group:
 C02N(H02T,H02U,H02V), C02Q(H02Z,H,HA)
;
_shelx_res_checksum              68939
_shelx_fab_checksum              34926
_olex2_submission_special_instructions 'No special instructions were received'