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_4122295
_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         '6(F6 P), C66 H54 N6, C4 H6 N2, 0.25(C36)'
_chemical_formula_sum            'C79 H66 F36 N8 P6'
_chemical_formula_weight         1997.21
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-06
_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                   18.1567(8)
_cell_length_b                   28.6627(13)
_cell_length_c                   21.1615(10)
_cell_measurement_reflns_used    7671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.82
_cell_measurement_theta_min      2.88
_cell_volume                     11012.9(9)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.989
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.923
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26346
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.73
_diffrn_reflns_theta_min         2.09
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.807
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0509 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.8460.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.716
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.443
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     876
_refine_ls_restrained_S_all      1.446
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0958
_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          0.3104
_refine_ls_wR_factor_ref         0.3321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3621
_reflns_number_total             4909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_010.cif
_cod_data_source_block           n2801
_cod_database_code               4122295
_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
 C35-C34 \\sim C33-C34 \\sim C32-C33 \\sim C31-C32 \\sim C30-C31 \\sim C30-C35 \\sim C30-C29 \\sim C28-C29
 \\sim C27-C28 \\sim C36-C27 \\sim C36-C35 \\sim C36-C37 \\sim C20-C37 \\sim C20-C25 \\sim C25-C26 \\sim C27-
 C26 \\sim C20-C21 \\sim C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C25-C24
 with sigma of 0.01
 P2-F7 \\sim P2-F7A \\sim P2-F9 \\sim P2-F9A \\sim P2-F10 \\sim P2-F8 \\sim P2-F9B
 with sigma of 0.02
3. Restrained planarity
 C36, C20, C21, C25, C37, C22, C24, C26, C23, C27, C35, C28, C30, C34, C29,
 C31, C33, C32
 with sigma of 0.1
4. Rigid bond restraints
 C26, C34, C33, C35, C32, C30, C36, C31, C29, C37, C27, C28, C20, C21, C25,
 C22, C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, F7A, F9, F9A, F9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C26 \\sim C34 \\sim C33 \\sim C35 \\sim C32 \\sim C30 \\sim C36 \\sim C31 \\sim C29 \\sim C37 \\sim C27 \\sim C28 \\sim C20 \\sim C21 \\sim C25 \\sim C22 \\sim C24 \\sim C23: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F7 \\sim F7A \\sim F9 \\sim F9A \\sim F9B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(F7A)=1-FVAR(1)
 Sof(F9A)=Sof(F9B)=0.5*(1-FVAR(2))
 Sof(F7)=Sof(F9)=FVAR(1)
 Fixed Sof: H(0.5) HA(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C20(0.125) C21(0.125)
 C22(0.125) C23(0.125) C24(0.125) C25(0.125) C26(0.125) C27(0.125) C28(0.125)
 C29(0.125) C30(0.125) C31(0.125) C32(0.125) C33(0.125) C34(0.125) C35(0.125)
 C36(0.125) C37(0.125)
7.a Secondary CH2 refined with riding coordinates:
 C3(H,HA), C16(H16A,H16B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19)
7.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_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.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 2456.7 Ang^3^ [22.3%]
Total electron count / cell = 475.8
;
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.660
_shelx_hkl_checksum              48914
_shelx_res_checksum              71067
_shelxl_version_number           2012-9