Supramolecular enantiomeric and structural differentiation of amino acid derivatives with achiral pillar[5]arene homologs.
Ji, Jiecheng; Li, Yizhou; Xiao, Chao; Cheng, Guo; Luo, Kui; Gong, Qiyong; Zhou, Dayang; Chruma, Jason J.; Wu, Wanhua; Yang, Cheng; Chemical communications (Cambridge, England) 56 (2020) 161–164; doi:10.1039/c9cc08541f

data_7125637
_publ_section_title
;
 Supramolecular enantiomeric and structural differentiation of amino acid
 derivatives with achiral pillar[5]arene homologs.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              161
_journal_page_last               164
_journal_paper_doi               10.1039/c9cc08541f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C105 H170 O10, C6 H4 N2'
_chemical_formula_sum            'C111 H174 N2 O10'
_chemical_formula_weight         1696.51
_chemical_name_systematic        H7-1
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                67.441(4)
_cell_angle_beta                 75.269(4)
_cell_angle_gamma                83.834(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9813(5)
_cell_length_b                   20.4770(8)
_cell_length_c                   22.1377(9)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7050
_cell_measurement_theta_min      3.7700
_cell_volume                     5255.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_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      1.00  77.00   1.00    1.00    --   39.71 -99.00 120.00   76
  2  \w     72.00 121.00   1.00    6.00    --  108.73-125.00  30.00   49
  3  \w     44.00 103.00   1.00    6.00    --  108.73 -94.00-120.00   59
  4  \w     92.00 121.00   1.00    6.00    --  108.73-125.00-150.00   29
  5  \w     40.00 139.00   1.00    6.00    --  108.73 -30.00   0.00   99
  6  \w     96.00 123.00   1.00    6.00    --  108.73  45.00-120.00   27
  7  \w    141.00 176.00   1.00    6.00    --  108.73 125.00 -60.00   35
  8  \w    108.00 135.00   1.00    6.00    --  108.73 125.00 -60.00   27
  9  \w     83.00 171.00   1.00    6.00    --  108.73  61.00  30.00   88
 10  \w     36.00 138.00   1.00    6.00    --  108.73 -61.00-120.00  102
 11  \w     33.00  83.00   1.00    1.00    --   39.71-125.00 -90.00   50
 12  \w     35.00  62.00   1.00    6.00    --  108.73-125.00-150.00   27
 13  \w     28.00 170.00   1.00    6.00    --  108.73 -15.00-150.00  142
 14  \w     34.00 106.00   1.00    6.00    --  108.73 -45.00 120.00   72
 15  \w     30.00 130.00   1.00    6.00    --  108.73 -77.00  30.00  100
 16  \w    -49.00 -12.00   1.00    1.00    --  -39.71 125.00   0.00   37
 17  \w    -81.00  -5.00   1.00    1.00    --  -39.71 125.00 -60.00   76
 18  \w   -115.00 -33.00   1.00    1.00    --  -39.71 -37.00 150.00   82
 19  \w   -117.00  -4.00   1.00    1.00    --  -39.71 -19.00-150.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0656127000
_diffrn_orient_matrix_UB_12      0.0083172000
_diffrn_orient_matrix_UB_13      -0.0710606000
_diffrn_orient_matrix_UB_21      -0.0653654000
_diffrn_orient_matrix_UB_22      0.0667148000
_diffrn_orient_matrix_UB_23      -0.0302834000
_diffrn_orient_matrix_UB_31      0.0805089000
_diffrn_orient_matrix_UB_32      0.0460180000
_diffrn_orient_matrix_UB_33      0.0059198000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36494
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.316
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         20670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0903
_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^)+(0.0927P)^2^+11.0434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2319
_refine_ls_wR_factor_ref         0.2612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13945
_reflns_number_total             20670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08541f2.cif
_cod_data_source_block           h7-1
_cod_depositor_comments
'Adding full bibliography for 7125634--7125637.cif.'
_cod_database_code               7125637
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.941
_reflns_odcompleteness_completeness 99.81
_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:
 C00N(H00a,H00b), C013(H01a,H01b), C014(H01c,H01d), C017(H01e,H01f), C018(H01g,
 H01h), C01A(H01i,H01j), C01B(H01k,H01l), C01C(H01m,H01n), C01D(H01o,H01p),
 C01E(H01q,H01r), C01F(H01s,H01t), C01G(H01u,H01v), C01H(H01w,H01x), C01I(H01y,
 H), C01J(H01z,Ha), C01K(H01,Hb), C01L(H0aa,Hc), C01M(H1aa,Hd), C01N(H2aa,He),
 C01O(H3aa,Hf), C01P(H4aa,Hg), C01Q(H5aa,Hh), C01R(H6aa,Hi), C01S(H7aa,Hj),
 C01T(H8aa,Hk), C01U(H9aa,Hl), C01V(H0ba,Hm), C01W(H1ba,Hn), C01X(H2ba,Ho),
 C01Y(H3ba,Hp), C01Z(H4ba,Hq), C020(H02a,H02b), C021(H02c,H02d), C022(H02e,
 H02f), C023(H02g,H02h), C024(H02i,H02j), C025(H02k,H02l), C026(H02m,H02n),
 C027(H02o,H02p), C028(H02q,H02r), C029(H02s,H02t), C02A(H02u,H02v), C02B(H02w,
 H02x), C02C(H02y,Hr), C02D(H02z,Hs), C02E(H02,Ht), C02F(H5ba,Hu), C02G(H6ba,
 Hv), C02H(H7ba,Hw), C02I(H8ba,Hx), C02J(H9ba,Hy), C02K(H0ca,Hz), C02N(H3ca,
 H9da), C02O(H4ca,H0ea), C02P(H5ca,H1ea), C02Q(H6ca,H2ea), C02S(H8ca,H5ea),
 C02V(H0da,H8ea), C02X(H2da,H1fa), C02Y(H3da,H2fa), C02Z(H4da,H3fa), C034(H03g,
 H03h), C037(H03l,H03m), C038(H03n,H03o), C03A(H03s,H03t)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00J(H00J), C00L(H00L), C00V(H00V), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C016(H016), C019(H019), C03C(H03x), C03D(H03y),
 C03E(H03z), C03F(H03)
2.c Idealised Me refined as rotating group:
 C02L(H1ca,H5da,H6da), C02M(H2ca,H7da,H8da), C02R(H7ca,H3ea,H4ea), C02T(H9ca,
 H6ea,H7ea), C02W(H1da,H9ea,H0fa), C030(H03a,H03b,H03c), C033(H03d,H03e,H03f),
 C035(H03i,H03j,H03k), C039(H03p,H03q,H03r), C03B(H03u,H03v,H03w)
;
_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 1.753
_oxdiff_exptl_absorpt_empirical_full_min 0.465