Ex2Box: Interdependent Modes of Binding in a Two-Nanometer-Long Synthetic Receptor
Michal Juríček; Jonathan C. Barnes; Edward J. Dale; Wei-Guang Liu; Nathan L. Strutt; Carson J. Bruns; Nicolaas A. Vermeulen; Kala C. Ghooray; Amy A. Sarjeant; Charlotte L. Stern; Youssry Y. Botros; William A. Goddard; J. Fraser Stoddart; Journal of the American Chemical Society 135 (2013) 12736–12746; doi:10.1021/ja4052763

data_4120379
_publ_section_title
;
 Ex2Box: Interdependent Modes of Binding in a Two-Nanometer-Long Synthetic
 Receptor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12736
_journal_page_last               12746
_journal_paper_doi               10.1021/ja4052763
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C60 H48 N4, 2(C16 H15 N3 O2), 4(F6 P), 2.5(C2 H3 N)'
_chemical_formula_sum            'C97 H85.5 F24 N12.5 O4 P4'
_chemical_formula_weight         2070.15
_chemical_name_systematic
;
 ?
;
_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             2013-03-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                81.1853(12)
_cell_angle_beta                 86.2716(13)
_cell_angle_gamma                64.9951(11)
_cell_formula_units_Z            1
_cell_length_a                   10.4059(3)
_cell_length_b                   11.3697(3)
_cell_length_c                   21.2021(5)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.24
_cell_volume                     2246.50(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            90082
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.047
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0678 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8995.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1063
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         13104
_refine_ls_number_restraints     1053
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.1051
_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^)+(0.1393P)^2^+6.2812P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2775
_refine_ls_wR_factor_ref         0.3111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8795
_reflns_number_total             13104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_012.cif
_cod_data_source_block           n2538
_cod_original_formula_sum        'C97 H85.50 F24 N12.50 O4 P4'
_cod_database_code               4120379
_cod_database_fobs_code          4120379
_olex2_refinement_description
;
1. others
 Fixed Sof: O1(0.5) O2(0.5) N3(0.5) N4(0.5) N5(0.5) C31(0.5) H31(0.5) C32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5) C36(0.5) C37(0.5)
 C38(0.5) H38(0.5) C39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5)
 H42(0.5) C43(0.5) C44(0.5) H44(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
 C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) O3(0.5) O4(0.5) N6(0.5) N7(0.5) N8(0.5)
 C47(0.5) H47(0.5) C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) C51(0.5)
 H51(0.5) C52(0.5) C53(0.5) C54(0.5) H54(0.5) C55(0.5) C56(0.5) H56(0.5)
 C57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5) C61(0.5)
 H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) N10(0.25)
 C63(0.25) C64(0.25) H64A(0.25) H64B(0.25) H64C(0.25)
 Fixed Uiso: H1A(0.035) H1B(0.035) H3(0.033) H4(0.033) H6(0.041) H7(0.04)
 H8A(0.036) H8B(0.036) H9(0.034) H10(0.031) H12(0.036) H13(0.036) H15(0.035)
 H16(0.036) H18(0.038) H19(0.037) H21(0.034) H22(0.033) H24(0.033) H25(0.033)
 H27(0.039) H28(0.039) H29(0.042) H30(0.042) H31(0.092) H33(0.084) H34(0.15)
 H35(0.146) H38(0.077) H40(0.072) H41(0.079) H42(0.079) H44(0.061) H45A(0.097)
 H45B(0.097) H45C(0.097) H46A(0.28) H46B(0.28) H46C(0.28) H47(0.07) H48(0.078)
 H49(0.079) H51(0.064) H54(0.063) H56(0.054) H58(0.045) H59(0.06) H60(0.072)
 H61A(0.173) H61B(0.173) H61C(0.173) H62A(0.095) H62B(0.095) H62C(0.095)
 H66A(0.08) H66B(0.08) H66C(0.08) H64A(0.352) H64B(0.352) H64C(0.352)
 Fixed X: H1A(0.4689) H1B(0.3007) H3(0.6223) H4(0.6449) H6(0.2199) H7(0.197)
 H8A(0.5356) H8B(0.3663) H9(0.6617) H10(0.6772) H12(0.2759) H13(0.2677)
 H15(0.7015) H16(0.7209) H18(0.2955) H19(0.2748) H21(0.7211) H22(0.7438)
 H24(0.353) H25(0.331) H27(0.7817) H28(0.799) H29(0.381) H30(0.3547)
 H31(0.6757) H33(0.4985) H34(0.2772) H35(0.2662) H38(0.5986) H40(0.6826)
 H41(0.7427) H42(0.588) H44(0.2884) H45A(0.7678) H45B(0.8836) H45C(0.7241)
 H46A(0.1833) H46B(0.1269) H46C(0.1431) H47(0.0709) H48(0.0568) H49(0.0732)
 H51(0.0072) H54(-0.0455) H56(0.0198) H58(-0.0277) H59(-0.0643) H60(-0.0292)
 H61A(0.0092) H61B(-0.0688) H61C(0.1003) H62A(-0.0041) H62B(0.0424) H62C(-
 0.1205) H66A(0.9758) H66B(1.0293) H66C(1.012) H64A(0.0177) H64B(0.0553)
 H64C(0.1758)
 Fixed Y: H1A(0.8703) H1B(0.9298) H3(0.6572) H4(0.4622) H6(0.6129) H7(0.8081)
 H8A(0.3248) H8B(0.3827) H9(0.4127) H10(0.4868) H12(0.5319) H13(0.4577)
 H15(0.4793) H16(0.5636) H18(0.7702) H19(0.6818) H21(0.7248) H22(0.816)
 H24(0.8544) H25(0.7621) H27(0.8277) H28(0.9406) H29(1.1089) H30(1.003)
 H31(1.0533) H33(1.2267) H34(1.2543) H35(1.1594) H38(0.9534) H40(0.8739)
 H41(0.7727) H42(0.7185) H44(0.8869) H45A(1.1235) H45B(1.1635) H45C(1.2709)
 H46A(0.8442) H46B(0.9154) H46C(0.7688) H47(0.9602) H48(0.7984) H49(0.603)
 H51(0.7704) H54(0.968) H56(1.3368) H58(1.3453) H59(1.1545) H60(1.0389)
 H61A(0.4874) H61B(0.4431) H61C(0.3899) H62A(1.6337) H62B(1.5017) H62C(1.5833)
 H66A(0.7284) H66B(0.6226) H66C(0.7691) H64A(1.2059) H64B(1.0609) H64C(1.1144)
 Fixed Z: H1A(0.987) H1B(0.9764) H3(0.9528) H4(0.9205) H6(0.8972) H7(0.9292)
 H8A(0.8914) H8B(0.8848) H9(0.8067) H10(0.7003) H12(0.6747) H13(0.7828)
 H15(0.6004) H16(0.496) H18(0.4871) H19(0.5921) H21(0.4232) H22(0.32)
 H24(0.2779) H25(0.3814) H27(0.2189) H28(0.1209) H29(0.102) H30(0.2005)
 H31(0.4124) H33(0.2456) H34(0.2853) H35(0.3892) H38(0.5163) H40(0.6257)
 H41(0.7292) H42(0.7967) H44(0.6593) H45A(0.2156) H45B(0.2406) H45C(0.228)
 H46A(0.7026) H46B(0.7647) H46C(0.7654) H47(0.3096) H48(0.257) H49(0.3183)
 H51(0.4783) H54(0.5238) H56(0.5062) H58(0.6988) H59(0.7056) H60(0.6209)
 H61A(0.3616) H61B(0.4219) H61C(0.4212) H62A(0.6225) H62B(0.6721) H62C(0.6518)
 H66A(0.9461) H66B(1.0087) H66C(1.0094) H64A(0.2474) H64B(0.2834) H64C(0.272)
;
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.918
_shelxl_version_number           2012-9