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_4126938
_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         'C65 H59 O10, C5.68'
_chemical_formula_sum            'C70.676 H59 O10'
_chemical_formula_weight         1068.36
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2017-08-10
_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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????
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_cell_angle_alpha                78.720(8)
_cell_angle_beta                 83.606(9)
_cell_angle_gamma                78.588(7)
_cell_formula_units_Z            2
_cell_length_a                   12.0426(17)
_cell_length_b                   13.8291(17)
_cell_length_c                   19.662(2)
_cell_measurement_reflns_used    6561
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3138.7(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      133
_diffrn_measured_fraction_theta_full 0.9733
_diffrn_measured_fraction_theta_max 0.9733
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40274
_diffrn_reflns_theta_full        27.6302
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.075
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.1303
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1126.0
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.6175
_refine_diff_density_rms         0.1140
_refine_ls_d_res_high            0.7663
_refine_ls_d_res_low             6.6804
_refine_ls_goodness_of_fit_ref   1.1495
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    99
_refine_ls_number_parameters     712
_refine_ls_number_reflns         14215
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.1491
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2958
_refine_ls_wR_factor_ref         0.3221
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8881
_reflns_number_total             14215
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2f
_cod_database_code               4126938
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C5-C6
 1.54 with sigma of 0.02
 C1-C6
 1.54 with sigma of 0.02
 C1-C4
 1.54 with sigma of 0.02
 C4-C3
 1.54 with sigma of 0.02
 C3-C2
 1.54 with sigma of 0.02
 C0aa-C5
 1.54 with sigma of 0.02
 C113-C151
 1.33 with sigma of 0.02
 C150-C149
 1.33 with sigma of 0.02
 C149-C141
 1.33 with sigma of 0.02
3. Others
 Fixed Sof: H2b(3.077)
4.a Secondary CH2 refined with riding coordinates:
 C46(H46a,H46b), C51(H51a,H51b), C57(H57a,H57b), C68(H68a,H68b), C77(H77a,
 H77b), C96(H96a,H96b), C99(H99a,H99b), C107(H10c,H10d), C112(H11a,H11b),
 C118(H11c,H11d), C124(H12a,H12b), C135(H13e,H13f), C141(H14a,H14b), C147(H14c,
 H14d)
4.b Aromatic/amide H refined with riding coordinates:
 C80(H80), C98(H98), C19(H19), C89(H89), C97(H97), C59(H59), C103(H103),
 C23(H23), C86(H86), C65(H65), C52(H52), C113(H113), C129(H129), C139(H139),
 C142(H142), C149(H149)
4.c X=CH2 refined with riding coordinates:
 C133(H13a,H13b), C101(H10a,H10b), C150(H15a,H15b), C134(H13c,H13d), C151(H15c,
 H15d)
4.d :
 C90(H90), C105(H105), C109(H109), C121(H121), C131(H131)
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_olex2_submission_special_instructions 'No special instructions were received'