Amphiphilic Perylene-Calix[4]arene Hybrids: Synthesis and Tunable Self-Assembly.
Rodler, Fabian; Schade, Boris; Jäger, Christof M; Backes, Susanne; Hampel, Frank; Böttcher, Christoph; Clark, Timothy; Hirsch, Andreas; Journal of the American Chemical Society 137 (2015) 3308–3317; doi:10.1021/ja512048t

data_4123484
_publ_section_title
;
 Amphiphilic Perylene-Calix[4]arene Hybrids: Synthesis and Tunable
 Self-Assembly.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3308
_journal_page_last               3317
_journal_paper_doi               10.1021/ja512048t
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C38 H40 O8'
_chemical_formula_sum            'C38 H40 O8'
_chemical_formula_weight         624.70
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_cell_angle_alpha                97.369(3)
_cell_angle_beta                 95.733(4)
_cell_angle_gamma                99.239(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7356(5)
_cell_length_b                   11.2251(4)
_cell_length_c                   14.6888(6)
_cell_measurement_reflns_used    6845
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      29.5616
_cell_measurement_theta_min      2.8123
_cell_volume                     1559.38(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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_temperature      173.00(14)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -10.00   28.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -      -10.5692  -97.0000  -33.0000 38

  2 omega   -6.00   50.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       12.2880  -97.0000  146.0000 56

  3 omega  -16.00   26.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       12.2880  -97.0000  105.0000 42

  4 omega  -10.00   84.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       12.2880   38.0000  -60.0000 94

  5 omega   20.00   46.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       12.2880  -97.0000  -33.0000 26

  6 omega  -40.00   63.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       12.2880    0.0000   90.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0261295000
_diffrn_orient_matrix_UB_12      0.0363001000
_diffrn_orient_matrix_UB_13      0.0432949000
_diffrn_orient_matrix_UB_21      -0.0660455000
_diffrn_orient_matrix_UB_22      -0.0155836000
_diffrn_orient_matrix_UB_23      0.0159168000
_diffrn_orient_matrix_UB_31      0.0220802000
_diffrn_orient_matrix_UB_32      -0.0512671000
_diffrn_orient_matrix_UB_33      0.0167168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15087
_diffrn_reflns_theta_full        29.63
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95096
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             664
_exptl_crystal_recrystallization_method 'crystallized from DCM'
_exptl_crystal_size_max          0.3557
_exptl_crystal_size_mid          0.2655
_exptl_crystal_size_min          0.2267
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.9022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                5948
_reflns_number_total             7362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja512048t_si_001.cif
_cod_data_source_block           fr01
_cod_depositor_comments          'Adding full bibliography for 4123484.cif.'
_cod_original_cell_volume        1559.39(12)
_cod_database_code               4123484
_chemical_oxdiff_formula         'C38 H40 O8'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C3(H3A), C4(H4), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C38(H38A,H38B,H38C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_olex2_date_sample_data_collection 1320685523.2
_olex2_date_sample_submission    26.10.2011
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_olex2_submission_special_instructions 'No special instructions were received'