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_4122292
_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, C14 H10, 6(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C86 H73 F36 N9 P6'
_chemical_formula_weight         2102.35
_chemical_name_systematic
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 ?
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-08
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1032(12)
_cell_length_b                   28.586(2)
_cell_length_c                   21.3729(13)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.92
_cell_measurement_theta_min      3.55
_cell_volume                     11060.4(13)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.993
_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  0.0833
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64749
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.71
_diffrn_reflns_theta_min         1.55
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0640 after correction.
The Ratio of minimum to maximum transmission is 0.8108.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         9709
_refine_ls_number_restraints     1657
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.1084
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3388
_refine_ls_wR_factor_ref         0.3714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5658
_reflns_number_total             9709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_008.cif
_cod_data_source_block           n2872
_cod_database_code               4122292
_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. Restrained distances
 C46-C45 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42 \\sim C47-C42 \\sim C47-C46 \\sim C47-C34 \\sim C39-C34
 \\sim C42-C41 \\sim C41-C40 \\sim C40-C39 \\sim C39-C38 \\sim C38-C37 \\sim C37-C36 \\sim C36-C35 \\sim C35-C34
 with sigma of 0.02
 C36-C39 \\sim C34-C37 \\sim C35-C38 \\sim C40-C47 \\sim C46-C43 \\sim C45-C42 \\sim C44-C47 \\sim C43-C46
 with sigma of 0.02
 C46A-C45A \\sim C45A-C44A \\sim C44A-C43A \\sim C43A-C42A \\sim C47A-C42A \\sim C47A-C46A \\sim C47A-
 C34A \\sim C39A-C34A \\sim C42A-C41A \\sim C41A-C40A \\sim C40A-C39A \\sim C39A-C38A \\sim C38A-C37A ~
 C37A-C36A \\sim C36A-C35A \\sim C35A-C34A
 with sigma of 0.02
 C36A-C39A \\sim C34A-C37A \\sim C35A-C38A \\sim C40A-C47A \\sim C46A-C43A \\sim C45A-C42A \\sim C44A-
 C47A \\sim C43A-C46A \\sim C34A-C41A \\sim C47A-C40A \\sim C39A-C42A
 with sigma of 0.02
 C35A-C47A \\sim C46A-C34A \\sim C43A-C41A \\sim C40A-C38A
 with sigma of 0.01
 P3-F18A \\sim P3-F14 \\sim P3-F14A \\sim P3-F16 \\sim P3-F16A \\sim P3-F13 \\sim P3-F13A \\sim P3-F18 ~
 P3-F17 \\sim P3-F15
 with sigma of 0.01
3. Rigid bond restraints
 C47, C34, C35, C39, C36, C38, C40, C42, C46, C37, C41, C43, C45, C44, C47A,
 C36A, C38A, C37A, C35A, C39A, C34A, C40A, C41A, C42A, C46A, C43A, C45A, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13A, F13, F18, F18A, F16A, F14, F14A, F16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C47 \\sim C34 \\sim C35 \\sim C39 \\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C46 \\sim C37 \\sim C41 \\sim C43 \\sim C45 \\sim C44 \\sim C47A \\sim C36A \\sim C38A \\sim C37A \\sim C35A \\sim C39A \\sim C34A \\sim C40A \\sim C41A \\sim C42A \\sim C46A \\sim C43A \\sim C45A \\sim C44A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F13A \\sim F13 \\sim F18 \\sim F18A \\sim F16A \\sim F14 \\sim F14A \\sim F16: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=
 Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=
 Sof(C42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=
 Sof(C46A)=Sof(H46A)=Sof(C47A)=0.5*(1-FVAR(2))
 Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=
 Sof(H38)=Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=0.5*
 FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F16A)=Sof(F18A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F16)=Sof(F18)=FVAR(2)
 Fixed Sof: N5(0.25) C50(0.25) C51(0.25) H(0.25) HA(0.25) HB(0.25) N6(0.25)
 C52(0.25) C53(0.25) HC(0.25) HD(0.25) HE(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C21(H21A,H21B), C30(H30A,H30B)
6.b Me refined with riding coordinates:
 C51(H,HA,HB), C53(HC,HD,HE)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C40A(H40A), C41A(H41A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A)
6.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
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_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 2169.3 Ang^3^ [19.8%]
Total electron count / cell = 263.5

The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.
;
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.621
_shelx_hkl_checksum              46698
_shelx_res_checksum              74257
_shelxl_version_number           2012-9