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_4122289
_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, C4 H6 N2, 6(F6 P)'
_chemical_formula_sum            'C70 H60 F36 N8 P6'
_chemical_formula_weight         1883.08
_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
_audit_creation_date             2013-05-13
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0422(7)
_cell_length_b                   28.4947(14)
_cell_length_c                   21.5301(7)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.303
_cell_measurement_theta_min      2.422
_cell_volume                     11068.8(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
;
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            183299
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         0.71
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0874 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.8725.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            '? light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00025(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.406
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.799
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0954
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3324
_refine_ls_wR_factor_ref         0.3527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4642
_reflns_number_total             6811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_003.cif
_cod_data_source_block           cmcm_2
_cod_database_code               4122289
_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
 F25-F21A \\sim F25-F23A \\sim F25-F25A_$1 \\sim F25-F25A \\sim F21A-F22A \\sim F21A-F25A_$1 -
 F21A-F25A \\sim F22A-F23A \\sim F22A-F25A_$1 \\sim F22A-F25A \\sim F23A-F25A_$1 \\sim F23A-F25A -
 F25A_$1-F25A
 with sigma of 0.04
 P2A-F25 \\sim P2A-F21A \\sim P2A-F22A \\sim P2A-F23A \\sim P2A-F25A_$1 \\sim P2A-F25A
 with sigma of 0.02
3. Others
 Sof(F25A)=1-FVAR(1)
 Sof(F25)=Sof(P2A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=0.5*(1-FVAR(2))
 Sof(P2)=Sof(F21)=Sof(F23)=0.5*FVAR(2)
 Sof(F22)=Sof(F24)=FVAR(1)
 Fixed Sof: H3A(0.5) H3B(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C16(H16A,H16B)
4.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), C17(H17), C19(H19)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
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_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.921
_shelx_hkl_checksum              13988
_shelx_res_checksum              84179
_shelxl_version_number           2013-3