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_4122293
_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, 6(F6 P), 0.5(C10 H8), 3(C2 H3 N) '
_chemical_formula_sum            'C77 H67 F36 N9 P6'
_chemical_formula_weight         1988.21
_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     dual
_audit_creation_date             2013-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0851(5)
_cell_length_b                   28.5005(8)
_cell_length_c                   21.5707(6)
_cell_measurement_reflns_used    9566
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.459
_cell_measurement_theta_min      3.546
_cell_volume                     11118.3(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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            95509
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.52
_diffrn_reflns_theta_min         2.05
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0737 before and 0.0437 after correction.
The Ratio of minimum to maximum transmission is 0.8537.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1769P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3183
_reflns_number_total             5324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_006.cif
_cod_data_source_block           n3148
_cod_database_code               4122293
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.522
_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
 C22-C23 \\sim C24-C23 \\sim C25-C24 \\sim C25-C20 \\sim C21-C20 \\sim C22-C21
 with sigma of 0.02
3. Rigid bond restraints
 F9A, F10, F12A, F9, F11A, F9, F12A, F10, F8, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C20, C25, C21, C24, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F9A \\sim F10 \\sim F12A \\sim F9 \\sim F11A \\sim F9 \\sim F12A \\sim F10
\\sim F8 \\sim F8A: within 1.7A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C23 \\sim C20 \\sim C25 \\sim C21 \\sim C24 \\sim C22: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F12A)=1-FVAR(1)
 Sof(F9A)=Sof(F11A)=0.5*(1-FVAR(2))
 Sof(F9)=Sof(F10)=FVAR(1)
 Sof(F8A)=0.5*(1-FVAR(3))
 Sof(F8)=0.5*FVAR(3)
 Fixed Sof: H(0.5) HA(0.5) C20(0.125) C21(0.125) C22(0.25) H22(0.25) C23(0.25)
 H23(0.25) C24(0.25) H24(0.25) C25(0.25) H25(0.25) HB(0.5) HC(0.5) HD(0.5)
 C29(0.25) C30(0.25) HE(0.25) HF(0.25) HG(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C3(H,HA), C16(H16A,H16B)
6.b Me refined with riding coordinates:
 C30(HE,HF,HG)
6.c 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), C22(H22), C23(H23), C24(H24), C25(H25)
6.d Idealised Me refined as rotating group:
 C27(HB,HC,HD)
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_smtbx_masks_special_details
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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 = 2713.0 Ang^3^ [24.4%]
Total electron count / cell = 673.8
;
_shelx_res_checksum              35684
_shelx_hkl_checksum              48672