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_4126937
_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         'C56 H58 Br5 O10, 0.5(C2 N2), C2 H3 N, C'
_chemical_formula_sum            'C60 H61 Br5 N2 O10'
_chemical_formula_weight         1346.86
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
????
;
_cell_angle_alpha                87.544(8)
_cell_angle_beta                 76.492(6)
_cell_angle_gamma                71.424(6)
_cell_formula_units_Z            2
_cell_length_a                   11.9944(10)
_cell_length_b                   12.9310(13)
_cell_length_c                   21.517(2)
_cell_measurement_reflns_used    7062
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3074.1(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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            33980
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.072
_exptl_absorpt_coefficient_mu    3.227
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2357
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.957
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         10744
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1460P)^2^+0.2300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7420
_reflns_number_total             10744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2e
_cod_database_code               4126937
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.046
_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. Restrained distances
 C56-Br1
 1.95 with sigma of 0.02
 C0AA-C1AA
 1.5 with sigma of 0.02
 C1AA-N9
 1.7 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C61(H61), C65(H65)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B), C16(H16A,H16B), C24(H24A,H24B),
 C25(H25A,H25B), C42(H42A,H42B), C43(H43A,H43B), C48(H48A,H48B), C49(H49A,H49B),
  C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C63(H63A,H63B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C17(H17), C18(H18), C21(H21), C31(H31), C39(H39),
 C46(H46), C47(H47), C51(H51), C62(H62)
3.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C59(H59A,H59B,
 H59C), C64(H64A,H64B,H64C), C0AA(H0AA,H0AB,H0AC)
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_olex2_submission_special_instructions 'No special instructions were received'