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_4126934
_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         'C55 H60 O10, C6 H14'
_chemical_formula_sum            'C61 H65 O10'
_chemical_formula_weight         958.13
_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     iterative
_audit_creation_date             2017-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
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_audit_update_record
;
????
;
_cell_angle_alpha                81.873
_cell_angle_beta                 76.172
_cell_angle_gamma                64.056
_cell_formula_units_Z            2
_cell_length_a                   11.8432
_cell_length_b                   12.2389
_cell_length_c                   21.2355
_cell_measurement_reflns_used    3622
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     2685.232
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      133
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28763
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.042
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1022
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0910P)^2^+0.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5654
_reflns_number_total             9360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2b
_cod_original_cell_volume        2685.2(6)
_cod_database_code               4126934
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C30(H30A,H30B), C33(H33A,H33B), C41(H41A,
 H41B), C44(H44A,H44B), C55(H55A,H55B), C59(H59A,H59B), C58(H58A,H58B),
 C57(H57A,H57B), C60(H60A,H60B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C9(H9), C15(H15), C18(H18), C20(H20), C26(H26), C29(H29),
 C31(H31), C37(H37), C40(H40), C42(H42), C48(H48), C51(H51), C53(H53)
2.c X=CH2 refined with riding coordinates:
 C43(H43A,H43B)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C34(H34A,H34B,
 H34C), C47(H47A,H47B,H47C), C61(H61A,H61B,H61C), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'