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_4126939
_publ_section_title
;
 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 H65 N15 O10'
_chemical_formula_sum            'C55 H65 N15 O10'
_chemical_formula_weight         1096.22
_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     direct
_audit_creation_date             2017-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r1)
;
_cell_angle_alpha                77.3250(16)
_cell_angle_beta                 80.6606(18)
_cell_angle_gamma                80.0120(16)
_cell_formula_units_Z            2
_cell_length_a                   12.6260(3)
_cell_length_b                   14.7182(2)
_cell_length_c                   17.3130(4)
_cell_measurement_reflns_used    43705
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      73.9370
_cell_measurement_theta_min      3.5640
_cell_volume                     3065.39(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -17.00 109.00   0.50    0.50    --   20.00  79.00 105.70  252
  2  \w    -17.00 109.00   0.50    0.50    --   20.00  78.00 -45.56  252
  3  \w    -57.00  62.00   0.50    0.50    --   32.00 -53.00  74.02  238
  4  \w     18.00 145.00   0.50    4.91    --   56.00  82.00  49.77  254
  5  \w     18.00 145.00   0.50    4.91    --   56.00  81.00 134.17  254
  6  \w     22.00 149.00   0.50    4.91    --   60.00  82.00 -76.68  254
  7  \w     22.00 149.00   0.50    4.91    --   60.00  82.00-111.60  254
  8  \w     22.00 149.00   0.50    4.91    --   60.00  82.00  -6.44  254
  9  \w     26.00 153.00   0.50    4.91    --   64.00  82.00 173.45  254
 10  \w     30.00 157.00   0.50    4.91    --   68.00  82.00 -63.44  254
 11  \w     38.00 165.00   0.50    4.91    --   76.00  81.00  54.44  254
 12  \w     38.00 165.00   0.50    4.91    --   76.00  82.00 125.95  254
 13  \w     38.00 165.00   0.50    4.91    --   76.00  81.00  91.62  254
 14  \w     38.00 165.00   0.50    4.91    --   76.00  81.00  23.78  254
 15  \w     42.00 169.00   0.50    4.91    --   80.00  82.00-173.49  254
 16  \w     42.00 169.00   0.50    4.91    --   80.00  81.00 -19.27  254
 17  \w     42.00 169.00   0.50    4.91    --   80.00  81.00 -19.27  254
 18  \w     46.00 173.00   0.50    4.91    --   84.00  82.00-135.02  254
 19  \w     46.00 173.00   0.50    4.91    --   84.00  82.00-159.82  254
 20  \w     54.00 177.00   0.50    4.91    --   88.00  71.00 173.42  246
 21  \w     60.00 188.00   0.50    4.91    --   98.20  82.00-120.00  256
 22  \w     62.00 188.00   0.50    4.91    --   98.20  77.00 -90.00  252
 23  \w     62.00 188.00   0.50    4.91    --   98.20  77.00 120.00  252
 24  \w     69.00 188.00   0.50    4.91    --   98.20  45.00 150.00  238
 25  \w      9.00 137.00   0.50    4.91    --   98.20 -82.00-120.00  256
 26  \w      9.00 137.00   0.50    4.91    --   98.20 -82.00 150.00  256
 27  \w     62.00 188.00   0.50    4.91    --   98.20  77.00   0.00  252
 28  \w     65.00 188.00   0.50    4.91    --   98.20  68.00-126.17  246
 29  \w      9.00 137.00   0.50    4.91    --   98.20 -82.00  90.00  256
 30  \w     60.00 188.00   0.50    4.91    --   98.20  82.00 -60.00  256
 31  \w     62.00 188.00   0.50    4.91    --   98.20  77.00  90.00  252
 32  \w     62.00 188.00   0.50    4.91    --   98.20  76.00  46.37  252
 33  \w     62.00 188.00   0.50    4.91    --   98.20  77.00-180.00  252
 34  \w      9.00 134.00   0.50    4.91    --   98.20 -30.00 -60.00  250
 35  \w      9.00 130.00   0.50    4.91    --   98.20 -61.00 150.00  242
 36  \w     60.00 188.00   0.50    4.91    --   98.20  82.00  60.00  256
 37  \w     60.00 188.00   0.50    4.91    --   98.20  82.00 -30.00  256
 38  \w     69.00 188.00   0.50    4.91    --   98.20  45.00   0.00  238
 39  \w     11.00 138.00   0.50    4.91    --  100.00 -82.00 -54.13  254
 40  \w     11.00 138.00   0.50    4.91    --  100.00 -82.00  -4.33  254
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279026000
_diffrn_orient_matrix_UB_12      -0.0237255000
_diffrn_orient_matrix_UB_13      0.0914803000
_diffrn_orient_matrix_UB_21      0.0171852000
_diffrn_orient_matrix_UB_22      -0.1055719000
_diffrn_orient_matrix_UB_23      -0.0025390000
_diffrn_orient_matrix_UB_31      0.1205668000
_diffrn_orient_matrix_UB_32      -0.0065264000
_diffrn_orient_matrix_UB_33      0.0092101000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            114440
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.769
_diffrn_reflns_theta_min         3.584
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160.0
_refine_diff_density_max         1.446
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         12179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1509P)^2^+1.6705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2473
_refine_ls_wR_factor_ref         0.2574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9653
_reflns_number_total             12179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10767_si_002.cif
_cod_data_source_block           T-P[5]_3
_cod_depositor_comments
;

2020-09-02
Z value changed, that in the original file is absurd
                 miguel
;
_cod_original_formula_units_Z            61
_cod_original_cell_volume        3065.40(11)
_cod_database_code               4126939
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C22(H22A,H22B), C25(H25A,H25B), C28(H28A,H28B), C33(H33A,H33B), C35(H35A,
 H35B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B),
 C46(H46A,H46B), C47(H47A,H47B), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,H54B),
  C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C66(H66A,
 H66B), C70(H70A,H70B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C23(H23), C24(H24), C29(H29), C30(H30),
 C31(H31), C32(H32), C37(H37)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C45(H45A,H45B,H45C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              17478
_shelx_hkl_checksum              73586
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.584