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_4120376
_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, C10 H6 N2 O4, 4(F6 P)'
_chemical_formula_sum            'C70 H54 F24 N6 O4 P4'
_chemical_formula_weight         1623.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-02-01
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9134(6)
_cell_length_b                   38.0668(17)
_cell_length_c                   12.1063(5)
_cell_measurement_reflns_used    1831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.99
_cell_measurement_theta_min      6.98
_cell_volume                     6872.8(5)
_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, Beta test 
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13018
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.756
_diffrn_reflns_theta_min         4.328
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0561 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8468.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0529P)^2^+6.5525P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2058
_reflns_number_total             3017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_009.cif
_cod_data_source_block           n2413
_cod_database_code               4120376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H23 of C23, H24 of C24, H25 of C25, H28 of C28, H29 of C29, H30 of C30, H1
  of C1, H2 of C2, H10 of C10, H5 of C5, {H15A,H15B} of C15, H17 of C17, H13 of
  C13, H14 of C14, H9 of C9, H6 of C6, {H20A,H20B} of C20, H18 of C18
2. Restrained distances
 C28-C27 - C29-C28 - C30-C29 - C30-C21 - C22-C21 - C27-C22 - C23-C22 - C24-C23
 - C25-C24 - C26-C25
 with sigma of 0.01
 N4-C26 - N3-C21
 with sigma of 0.01
 O4-N4 - O3-N4 - O1-N3 - O2-N3
 with sigma of 0.01
 C21-C28 - C29-C22 - C27-C30 - C23-C26 - C25-C22 - C27-C24
 with sigma of 0.01
 O4-O3 - O1-O2
 with sigma of 0.01
3. Rigid bond restraints
 C28, C22, C21, C23, C27, C30, N3, C24, C26, C29, O1, O2, C25, N4, O4, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C28 - C22 - C21 - C23 - C27 - C30 - N3 - C24 - C26 - C29 - O1 - O2 - C25 - N4 
- O4 - O3: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) - Ueq, Uanis(O2) - Ueq, Uanis(O3) - Ueq, Uanis(O4) - Ueq: with sigma 
of 0.01 and sigma for terminal atoms of 0.02
5. others
 Fixed Sof: H15A(0.5) H15B(0.5) H20A(0.5) H20B(0.5) O1(0.25) O2(0.25) O3(0.25)
 O4(0.25) N3(0.25) N4(0.25) C21(0.25) C22(0.25) C23(0.25) H23(0.25) C24(0.25)
 H24(0.25) C25(0.25) H25(0.25) C26(0.25) C27(0.25) C28(0.25) H28(0.25)
 C29(0.25) H29(0.25) C30(0.25) H30(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14),
 C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30)
;
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.698
_shelx_res_checksum              7987
_shelxl_version_number           2012-9