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_4126933
_publ_section_title
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 Rim-Differentiated C5-Symmetric Tiara-Pillar[5]arenes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10767
_journal_year                    2017
_chemical_formula_moiety         'C55 H40 O10, C6 H14'
_chemical_formula_sum            'C61 H64 O10'
_chemical_formula_weight         957.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r1)
;
_audit_update_record
;
????
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_cell_angle_alpha                90
_cell_angle_beta                 90.104(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.719(2)
_cell_length_b                   14.849(2)
_cell_length_c                   35.106(3)
_cell_measurement_reflns_used    8571
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     10279.3(19)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9418
              2theta: -15.0639
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9418
              2theta: -15.0639
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9418
              2theta: -15.0639
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.000540
_diffrn_orient_matrix_UB_12      0.079088
_diffrn_orient_matrix_UB_13      0.029075
_diffrn_orient_matrix_UB_21      -0.079480
_diffrn_orient_matrix_UB_22      0.027574
_diffrn_orient_matrix_UB_23      -0.006001
_diffrn_orient_matrix_UB_31      -0.005355
_diffrn_orient_matrix_UB_32      -0.009661
_diffrn_orient_matrix_UB_33      0.026256
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            64336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         3.110
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4080
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         11832
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0750P)^2^+14.3957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8387
_reflns_number_total             11832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_2a
_cod_depositor_comments
;
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        10279(2)
_cod_database_code               4126933
_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. Shared sites
{C43, C43'}
{C46, C46'}
{C49, C49'}
{C52, C52'}
{C55, C55'}
3. Restrained distances
 C61-C60
 1.5 with sigma of 0.02
 C56-C57
 1.5 with sigma of 0.02
 C60-C61
 1.5 with sigma of 0.02
 C60-C59
 1.5 with sigma of 0.02
 C59-C58
 1.5 with sigma of 0.02
 C58-C57
 1.5 with sigma of 0.02
 C57-C56
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C43')
Uanis(C46) = Uanis(C46')
Uanis(C49) = Uanis(C49')
Uanis(C52) = Uanis(C52')
Uanis(C55) = Uanis(C55')
5. Others
 Fixed Sof: O6(0.5) O6'(0.5) O7(0.5) O7'(0.5) O8(0.5) O8'(0.5) O9(0.5)
 O9'(0.5) O10(0.5) O10'(0.5) C41(0.5) H41A(0.5) H41B(0.5) C41'(0.5) H41C(0.5)
 H41D(0.5) C42(0.5) C42'(0.5) C44(0.5) H44A(0.5) H44B(0.5) C44'(0.5) H44C(0.5)
 H44D(0.5) C45(0.5) C45'(0.5) C43(0.5) H43(0.5) C46(0.5) H46(0.5) C49(0.5)
 H49(0.5) C52(0.5) H52(0.5) C55(0.5) H55(0.5) C43'(0.5) H43'(0.5) C46'(0.5)
 H46'(0.5) C49'(0.5) H49'(0.5) C52'(0.5) H52'(0.5) C55'(0.5) H55'(0.5) C47(0.5)
 H47A(0.5) H47B(0.5) C47'(0.5) H47C(0.5) H47D(0.5) C48(0.5) C48'(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) C50'(0.5) H50C(0.5) H50D(0.5) C51(0.5) C51'(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) C53'(0.5) H53C(0.5) H53D(0.5) C54(0.5) C54'(0.5) O1(0.5)
 O2(0.5) O3(0.5) O4(0.5) O5(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
 C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5)
 C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
 O1'(0.5) O2'(0.5) O3'(0.5) O4'(0.5) O5'(0.5) C36'(0.5) H36D(0.5) H36E(0.5)
 H36F(0.5) C37'(0.5) H37D(0.5) H37E(0.5) H37F(0.5) C38'(0.5) H38D(0.5)
 H38E(0.5) H38F(0.5) C39'(0.5) H39D(0.5) H39E(0.5) H39F(0.5) C40'(0.5)
 H40D(0.5) H40E(0.5) H40F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C35(H35A,H35B),
 C41(H41A,H41B), C41'(H41C,H41D), C44(H44A,H44B), C44'(H44C,H44D), C47(H47A,
 H47B), C47'(H47C,H47D), C50(H50A,H50B), C50'(H50C,H50D), C53(H53A,H53B),
 C53'(H53C,H53D), C60(H60A,H60B), C59(H59A,H59B), C58(H58A,H58B), C57(H57A,H57B)
6.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C36'(H36D,H36E,H36F), C37'(H37D,H37E,H37F),
 C38'(H38D,H38E,H38F), C39'(H39D,H39E,H39F), C40'(H40D,H40E,H40F), C61(H61A,
 H61B,H61C), C56(H56A,H56B,H56C)
6.c :
 C43(H43), C46(H46), C49(H49), C52(H52), C55(H55), C43'(H43'), C46'(H46'),
 C49'(H49'), C52'(H52'), C55'(H55')
;
_shelx_res_checksum              13440
_shelx_hkl_checksum              44853
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'