Synthesis, Structure, and Properties of Corona[6]arenes and Their Assembly with Anions in the Crystalline State.
Zhao, Meng-Yao; Wang, De-Xian; Wang, Mei-Xiang; The Journal of organic chemistry 83 (2018) 1502–1509; doi:10.1021/acs.joc.7b03136

data_4033392
_publ_section_title
;
 Synthesis, Structure, and Properties of Corona[6]arenes and Their
 Assembly with Anions in the Crystalline State.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1502
_journal_page_last               1509
_journal_paper_doi               10.1021/acs.joc.7b03136
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety
'2(C32 H22 N10 O6), 2(C16 H36 N), C10 H6 O6 S2, 4(C2 H6 O S), C4 H10 O'
_chemical_formula_sum            'C118 H156 N22 O23 S6'
_chemical_formula_weight         2443.00
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
????
;
_cell_angle_alpha                100.163(4)
_cell_angle_beta                 92.151(5)
_cell_angle_gamma                96.439(5)
_cell_formula_units_Z            1
_cell_length_a                   11.713(3)
_cell_length_b                   12.688(4)
_cell_length_c                   21.381(6)
_cell_measurement_reflns_used    8596
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4826
_cell_measurement_theta_min      1.6426
_cell_volume                     3102.6(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36273
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.643
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         11130
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0923P)^2^+3.5911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9330
_reflns_number_total             11130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b03136_si_011.cif
_cod_data_source_block           mx6115
_cod_depositor_comments
'Adding full bibliography for 4033391--4033399.cif.'
_cod_database_code               4033392
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.949
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S2A-C60A = S2A-C59
 1.82 with sigma of 0.01
 S1A-C58A = S1A-C57A
 1.82 with sigma of 0.01
 S1-C57 = S1-C58 = S2-C59 = S2-C60
 1.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1A \\sim S1 \\sim O12 \\sim C57 \\sim C58 \\sim C58A \\sim C57A: within 1.9A
with sigma of 0.02 and sigma for terminal atoms of 0.04
C60A \\sim S2 \\sim O11 \\sim C59 \\sim C60 \\sim S2A: within 1.9A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C55 \\sim O10 \\sim C56: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(O12) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C57A) \\sim Ueq,
Uanis(C60A) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(S2A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=
 Sof(S2A)=1-FVAR(1)
 Sof(S2)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=
 FVAR(1)
 Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C58A)=Sof(H58D)=Sof(H58E)=
 Sof(H58F)=Sof(S1A)=1-FVAR(2)
 Sof(S1)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=FVAR(2)
5.a Riding coordinates:
 C45(H45A,H45B,H45C), C60A(H60D,H60E,H60F)
5.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B)
5.c Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C59(H59D,H59E,H59F)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C29(H29), C31(H31), C32(H32),
  C34(H34), C36(H36), C37(H37)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C41(H41A,H41B,H41C), C50(H50A,H50B,
 H50C), C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C57(H57A,H57B,H57C), C55(H55A,
 H55B,H55C), C58(H58A,H58B,H58C), C57A(H57D,H57E,H57F), C58A(H58D,H58E,H58F)
;
_shelx_res_checksum              11304
_shelx_hkl_checksum              80793
_olex2_submission_special_instructions 'No special instructions were received'