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_4126936
_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         'C50 H50 Br5 O10, C6 H13'
_chemical_formula_sum            'C56 H63 Br5 O10'
_chemical_formula_weight         1294.05
_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     direct
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                86.437(6)
_cell_angle_beta                 79.558(6)
_cell_angle_gamma                78.681(6)
_cell_formula_units_Z            2
_cell_length_a                   12.2345(13)
_cell_length_b                   14.0997(17)
_cell_length_c                   16.955(2)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    133
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      3.122
_cell_volume                     2819.3(6)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      133
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31210
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.122
_exptl_absorpt_coefficient_mu    3.605
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2150
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1004P)^2^+2.9092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6920
_reflns_number_total             9855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2d
_cod_original_cell_volume        2819.4(6)
_cod_database_code               4126936
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.047
_shelx_estimated_absorpt_t_min   0.065
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H20A,H20B} of C20, {H26A,H26B} of C26, {H27A,H27B} of C27,
   {H57A,H57B} of C57, {H58A,H58B} of C58, {H61A,H61B} of C61, {H62A,H62B} of
  C62, {H2A,H2B} of C2, {H46A,H46B} of C46, {H45A,H45B} of C45, {H42A,H42B} of
  C42, {H51A,H51B} of C51, {H49A,H49B} of C49, {H8A,H8B} of C8, {H16A,H16B} of
  C16
 At 1.5 times of:
  All C(H,H,H) groups, {H53A,H53B} of C53
2. Restrained distances
 C1-C2
 1.5 with sigma of 0.02
 C2-C66
 1.5 with sigma of 0.02
 C66-C65
 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
 C63-C62
 1.5 with sigma of 0.02
 C62-C61
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: C61(0.5) C62(0.5) C66(0.5) C1(0.5) C2(0.5) C67(0.5)
4.a Ternary CH refined with riding coordinates:
 C60(H60)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C20(H20A,H20B), C26(H26A,H26B), C27(H27A,H27B),
 C42(H42A,H42B), C45(H45A,H45B), C46(H46A,H46B), C49(H49A,H49B), C51(H51A,H51B),
  C57(H57A,H57B), C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C18(H18), C32(H32), C37(H37), C38(H38), C40(H40),
 C43(H43), C48(H48), C50(H50), C56(H56), C63(H63), C64(H64), C65(H65), C66(H66)
4.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C67(H67A,H67B,H67C)
;
_olex2_submission_special_instructions 'No special instructions were received'