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_4126940
_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 H50 O10, C6'
_chemical_formula_sum            'C61 H50 O10'
_chemical_formula_weight         943.01
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-22
_audit_creation_method
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_audit_update_record
;
????
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_cell_angle_alpha                90
_cell_angle_beta                 98.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9755(18)
_cell_length_b                   12.7943(12)
_cell_length_c                   21.464(2)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5150.8(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      133
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44142
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         3.110
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.9836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1984.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         9076
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1026P)^2^+4.7228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7083
_reflns_number_total             9076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           P[5]_S5
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5150.9(9)
_cod_database_code               4126940
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.984
_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
 C56-C58 = C57-C59 = C58-C60 = C59-C61
 2.5 with sigma of 0.01
 C56'-C58' = C57'-C59' = C58'-C60' = C59'-C61'
 2.5 with sigma of 0.01
 C56-C57 = C57-C58 = C58-C59 = C59-C60 = C60-C61
 1.54 with sigma of 0.01
 C56'-C57' = C57'-C58' = C58'-C59' = C59'-C60' = C60'-C61'
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C56' \\sim C57'
\\sim C58' \\sim C59' \\sim C60' \\sim C61': within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C56') \\sim Ueq,
Uanis(C57') \\sim Ueq, Uanis(C58') \\sim Ueq, Uanis(C59') \\sim Ueq,
Uanis(C60') \\sim Ueq, Uanis(C61') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C56')=Sof(C57')=Sof(C58')=Sof(C59')=Sof(C60')=Sof(C61')=1-FVAR(1)
 Sof(C56)=Sof(C57)=Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C12(H12A,H12B), C19(H19A,H19B), C23(H23A,H23B),
 C30(H30A,H30B), C34(H34A,H34B), C41(H41A,H41B), C45(H45A,H45B), C52(H52A,H52B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C18(H18), C25(H25), C28(H28), C36(H36), C39(H39),
 C47(H47), C50(H50)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C44(H44A,H44B,
 H44C), C55(H55A,H55B,H55C)
5.d :
 C10(H10), C21(H21), C32(H32), C43(H43), C54(H54)
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_olex2_submission_special_instructions 'No special instructions were received'