ExCage
Dale, Edward J.; Vermeulen, Nicolaas A.; Thomas, Andy A.; Barnes, Jonathan C.; Juríček, Michal; Blackburn, Anthea K.; Strutt, Nathan L.; Sarjeant, Amy A.; Stern, Charlotte L.; Denmark, Scott E.; Stoddart, J. Fraser; Journal of the American Chemical Society 136 (2014) 10669–; doi:10.1021/ja5041557

data_4122290
_publ_section_title
;
 ExCage
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10669
_journal_paper_doi               10.1021/ja5041557
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C66 H54 N6, C18 H12, 6(F6 P), 7(C2 H3 N)'
_chemical_formula_sum            'C98 H115 F36 N13 P6'
_chemical_formula_weight         2344.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2013-07-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2677(8)
_cell_length_b                   30.7383(12)
_cell_length_c                   21.5011(9)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.74
_cell_measurement_theta_min      2.88
_cell_volume                     11256.8(8)
_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
;
SHELXD, 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 0.980
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77915
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.04
_diffrn_reflns_theta_min         1.44
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8509.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         19974
_refine_ls_number_restraints     1621
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0933
_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^)+(0.1100P)^2^+40.0874P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2456
_refine_ls_wR_factor_ref         0.2529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16496
_reflns_number_total             19974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_005.cif
_cod_data_source_block           n2871
_cod_database_code               4122290
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F25A-F26A \\sim F25A-F28A \\sim F25A-F29A \\sim F25A-F30A \\sim F26A-F27A 
 \\sim F26A-F29A \\sim F26A-
 F30A \\sim F27A-F28A \\sim F27A-F29A \\sim F27A-F30A \\sim F28A-F29A 
 \\sim F28A-F30A
 with sigma of 0.04
 P5A-F25A \\sim P5A-F26A \\sim P5A-F27A \\sim P5A-F28A \\sim P5A-F29A 
 \\sim P5A-F30A
 with sigma of 0.02
 F25-F26 \\sim F25-F28 \\sim F25-F29 \\sim F25-F30 \\sim F26-F27 \\sim F26-F29 
 \\sim F26-F30 \\sim F27-F28
 \\sim F27-F29 \\sim F27-F30 \\sim F28-F29 \\sim F28-F30
 with sigma of 0.04
 P5-F25 \\sim P5-F26 \\sim P5-F27 \\sim P5-F28 \\sim P5-F29 \\sim P5-F30
 with sigma of 0.02
 C84-C67 \\sim C68-C67 \\sim C69-C68 \\sim C70-C69 \\sim C71-C70 \\sim C84-C71 
 \\sim C72-C71 \\sim C73-C72
 \\sim C74-C73 \\sim C83-C74 \\sim C84-C83 \\sim C75-C74 \\sim C76-C75 
 \\sim C77-C76 \\sim C82-C77 \\sim C83-
 C82 \\sim C78-C77 \\sim C79-C78 \\sim C80-C79 \\sim C81-C80 \\sim C82-C81 
 \\sim C84A-C67A \\sim C68A-C67A
 \\sim C69A-C68A \\sim C70A-C69A \\sim C71A-C70A \\sim C84A-C71A 
 \\sim C72A-C71A \\sim C73A-C72A \\sim C74A-
 C73A \\sim C83A-C74A \\sim C84A-C83A \\sim C75A-C74A \\sim C76A-C75A 
 \\sim C77A-C76A \\sim C82A-C77A ~
 C83A-C82A \\sim C78A-C77A \\sim C79A-C78A \\sim C80A-C79A \\sim C81A-C80A 
 \\sim C82A-C81A
 with sigma of 0.02
 C67-C69 \\sim C68-C70 \\sim C71-C73 \\sim C72-C74 \\sim C83-C75 \\sim C76-C82 
 \\sim C77-C81 \\sim C80-C78
 \\sim C84-C68 \\sim C79-C81 \\sim C79-C81 \\sim C67-C69 \\sim C67A-C69A 
 \\sim C68A-C70A \\sim C71A-C73A ~
 C72A-C74A \\sim C83A-C75A \\sim C76A-C82A \\sim C77A-C81A \\sim C80A-C78A 
 \\sim C84A-C68A \\sim C79A-
 C81A \\sim C79A-C81A \\sim C67A-C69A
 with sigma of 0.02
 C68-C71 \\sim C67-C70 \\sim C69-C84 \\sim C72-C83 \\sim C74-C77 \\sim C75-C82
 \\sim C81-C78 \\sim C84-C73
 \\sim C76-C83 \\sim C80-C77 \\sim C79-C82 \\sim C68A-C71A \\sim C67A-C70A 
 \\sim C69A-C84A \\sim C72A-C83A
 \\sim C74A-C77A \\sim C75A-C82A \\sim C81A-C78A \\sim C84A-C73A 
 \\sim C76A-C83A \\sim C80A-C77A \\sim C79A-
 C82A
 with sigma of 0.02
3. Rigid bond restraints
 C73, C67, C68, C84, C69, C71, C83, C70, C72, C74, C82, C75, C77, C81, C76,
 C78, C80, C79
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C73 \\sim C67 \\sim C68 \\sim C84 \\sim C69 \\sim C71 \\sim C83 \\sim C70 
\\sim C72 \\sim C74 \\sim C82 \\sim C75 \\sim C77 \\sim C81 \\sim C76 \\sim C78
 \\sim C80 \\sim C79: within 1.7A with sigma of 0.04 and sigma for terminal
 atoms of 0.08
Uanis(C69A) = Uanis(C67A) = Uanis(C68A) = Uanis(C84A) = Uanis(C71A) = 
Uanis(C83A) = Uanis(C70A) = Uanis(C72A) = Uanis(C74A) = Uanis(C82A) = 
Uanis(C73A) = Uanis(C75A) = Uanis(C77A) = Uanis(C81A) = Uanis(C76A) = 
Uanis(C78A) = Uanis(C80A) = Uanis(C79A)
5. Others
 Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=
 Sof(H70A)=Sof(C71A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=
 Sof(C75A)=Sof(H75A)=Sof(C76A)=Sof(H76A)=Sof(C77A)=Sof(C78A)=Sof(H78A)=
 Sof(C79A)=Sof(H79A)=Sof(C80A)=Sof(H80A)=Sof(C81A)=Sof(H81A)=Sof(C82A)=
 Sof(C83A)=Sof(C84A)=1-FVAR(1)
 Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=
 Sof(C71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(C75)=Sof(H75)=
 Sof(C76)=Sof(H76)=Sof(C77)=Sof(C78)=Sof(H78)=Sof(C79)=Sof(H79)=Sof(C80)=
 Sof(H80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(C83)=Sof(C84)=FVAR(1)
 Sof(F32A)=Sof(F33A)=Sof(F31A)=Sof(F35A)=Sof(F36A)=Sof(F34A)=1-FVAR(2)
 Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=FVAR(2)
 Sof(P5A)=Sof(F25A)=Sof(F26A)=Sof(F27A)=Sof(F28A)=Sof(F29A)=Sof(F30A)=1-FVAR(3)
 Sof(P5)=Sof(F25)=Sof(F26)=Sof(F27)=Sof(F28)=Sof(F29)=Sof(F30)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C29(H29A,H29B), C36(H36A,H36B), C43(H43A,H43B), C60(H60A,
 H60B), C66(H66A,H66B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35), C38(H38),
 C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50),
  C52(H52), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C62(H62),
 C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72),
  C73(H73), C75(H75), C76(H76), C78(H78), C79(H79), C80(H80), C81(H81),
 C67A(H67A), C68A(H68A), C69A(H69A), C70A(H70A), C72A(H72A), C73A(H73A),
 C75A(H75A), C76A(H76A), C78A(H78A), C79A(H79A), C80A(H80A), C81A(H81A)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  The formula
reported here reflects the 28 acetonitrile molecules removed by this treatment.

Total solvent accessible volume / cell = 3605.0 Ang^3 [32.0%]
Total electron count / cell = 642.8
;
_shelxl_version_number           2012-9