Rim-Differentiated C5-Symmetric Tiara-Pillar[5]arenes.
Guo, Minjie; Wang, Xuemei; Zhan, Caihong; Demay-Drouhard, Paul; Li, Wenjiao; Du, Ke; Olson, Mark A.; Zuilhof, Han; Sue, Andrew C.-H.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10767

data_4126935
_publ_section_title
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 Rim-Differentiated C5-Symmetric Tiara-Pillar[5]arenes.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10767
_journal_year                    2017
_chemical_formula_moiety         'C60 H70 O10, C6 H14'
_chemical_formula_sum            'C66 H84 O10'
_chemical_formula_weight         1037.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-02
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
;
????
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3445(10)
_cell_length_b                   20.6410(15)
_cell_length_c                   23.2546(18)
_cell_measurement_reflns_used    11439
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5925.3(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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Pilatus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            76180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.647
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
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_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         13608
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0656P)^2^+0.7722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                10710
_reflns_number_total             13608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2c
_cod_database_code               4126935
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
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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. Restrained distances
 C60'-C61'
 1.5 with sigma of 0.02
 C62'-C63'
 1.5 with sigma of 0.02
 C63'-C64'
 1.5 with sigma of 0.02
 C64'-C65'
 1.5 with sigma of 0.02
 C61'-C62'
 1.5 with sigma of 0.02
 C63'-C62'
 1.5 with sigma of 0.02
 C65-C64
 1.5 with sigma of 0.02
 C64-C63
 1.5 with sigma of 0.02
 C61-C60
 1.5 with sigma of 0.02
 C61-C62
 1.5 with sigma of 0.02
 C62-C63
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C62) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5)
 H45(0.5) C46(0.5) H46A(0.5) H46B(0.5) C43'(0.5) H43C(0.5) H43D(0.5) C44'(0.5)
 H44C(0.5) H44D(0.5) C45'(0.5) H45'(0.5) C46'(0.5) H46C(0.5) H46D(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C65(0.5)
 H65A(0.5) H65B(0.5) H65C(0.5) C60'(0.5) H60D(0.5) H60E(0.5) H60F(0.5)
 C61'(0.5) H61C(0.5) H61D(0.5) C62'(0.5) H62C(0.5) H62D(0.5) C63'(0.5)
 H63C(0.5) H63D(0.5) C64'(0.5) H64C(0.5) H64D(0.5) C65'(0.5) H65D(0.5)
 H65E(0.5) H65F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B),
 C23(H23A,H23B), C31(H31A,H31B), C32(H32A,H32B), C35(H35A,H35B), C47(H47A,H47B),
  C55(H55A,H55B), C56(H56A,H56B), C59(H59A,H59B), C43(H43A,H43B), C44(H44A,
 H44B), C43'(H43C,H43D), C44'(H44C,H44D), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C61'(H61C,H61D), C62'(H62C,H62D), C63'(H63C,
 H63D), C64'(H64C,H64D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C14(H14), C17(H17), C21(H21), C25(H25), C28(H28),
 C33(H33), C37(H37), C40(H40), C49(H49), C52(H52), C57(H57), C45(H45),
 C45'(H45')
5.c X=CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C34(H34A,H34B), C58(H58A,H58B), C46(H46A,
 H46B), C46'(H46C,H46D)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C42(H42A,H42B,
 H42C), C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C),
 C60'(H60D,H60E,H60F), C65'(H65D,H65E,H65F)
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_shelx_res_checksum              8768
_shelx_hkl_checksum              91189
_olex2_submission_special_instructions 'No special instructions were received'