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_4122291
_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, C24 H12, 6(F6 P)'
_chemical_formula_sum            'C90 H66 F36 N6 P6'
_chemical_formula_weight         2101.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2014-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 120.757(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1338(18)
_cell_length_b                   30.560(2)
_cell_length_c                   18.2064(11)
_cell_measurement_reflns_used    702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.306
_cell_measurement_theta_min      4.044
_cell_volume                     11060.9(14)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8262
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        50.420
_diffrn_reflns_theta_max         50.424
_diffrn_reflns_theta_min         2.651
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.534259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0909 before and 0.0380 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0851 before and 0.0380 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.1026 before and 0.0394 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 26007 reflections, Rint = 0.0750
 (5792 with I > 3sig(I), Rint = 0.0520)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       rod
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         8262
_refine_ls_number_restraints     1851
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.1118
_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          0.2989
_refine_ls_wR_factor_ref         0.3381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5354
_reflns_number_total             8262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_004.cif
_cod_data_source_block           n2882_sq_s
_cod_original_cell_volume        11061.0(15)
_cod_database_code               4122291
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.637
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F7-F8 \\sim F7-F10 \\sim F7-F11 \\sim F7-F12 \\sim F8-F9 \\sim F8-F11 \\sim
F8-F12 \\sim F9-F10 \\sim F9-F11
 \\sim F9-F12 \\sim F10-F11 \\sim F10-F12
 with sigma of 0.04
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.02
 F7A-F8A \\sim F7A-F10A \\sim F7A-F11A \\sim F7A-F12A \\sim F8A-F9A \\sim
F8A-F11A \\sim F8A-F12A ~
 F9A-F10A \\sim F9A-F11A \\sim F9A-F12A \\sim F10A-F11A \\sim F10A-F12A
 with sigma of 0.04
 P2A-F7A \\sim P2A-F8A \\sim P2A-F9A \\sim P2A-F10A \\sim P2A-F11A \\sim
P2A-F12A
 with sigma of 0.02
 C40-C39 \\sim C41-C40 \\sim C42-C41 \\sim C43-C42 \\sim C44-C43 \\sim C45-C44
\\sim C46-C45 \\sim C47-C46
 \\sim C48-C47 \\sim C49-C48 \\sim C50-C49 \\sim C51-C50 \\sim C52-C51 \\sim
C53-C52 \\sim C54-C53 \\sim C55-
 C54 \\sim C55-C38 \\sim C39-C38 \\sim C56-C38 \\sim C57-C41 \\sim C58-C44
\\sim C47-C1A \\sim C59-C50 ~
 C60-C53 \\sim C60-C59 \\sim C60-C56 \\sim C57-C56 \\sim C58-C57 \\sim C58-C1A
\\sim C59-C1A
 with sigma of 0.02
3. Rigid bond restraints
 C45, C48, C47, C49, C46, C1A, C50, C58, C59, C51, C44, C57, C60, C52, C43,
 C41, C56, C53, C42, C40, C38, C54, C39, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, F7, F8, F9, F10, F11, F12, P2A, F9A, F7A, F8A, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C45 \\sim C48 \\sim C47 \\sim C49 \\sim C46 \\sim C1A \\sim C50 \\sim C58 \\sim
C59 \\sim C51 \\sim C44 \\sim C57 \\sim C60 \\sim C52 \\sim C43 \\sim C41 \\sim
C56 \\sim C53 \\sim C42 \\sim C40 \\sim C38 \\sim C54 \\sim C39 \\sim C55:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
P2 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim P2A \\sim F9A
\\sim F7A \\sim F8A \\sim F10A \\sim F11A \\sim F12A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Fixed Sof: H13A(0.5) H13B(0.5) H18A(0.5) H18B(0.5) C48(0.5) H48(0.5) C47(0.5)
 C46(0.5) H46(0.5) C45(0.5) H45(0.5) C44(0.5) C43(0.5) H43(0.5) C42(0.5)
 H42(0.5) C41(0.5) C49(0.5) H49(0.5) C1A(0.5) C58(0.5) C57(0.5) C40(0.5)
 H40(0.5) C39(0.5) H39(0.5) C38(0.5) C55(0.5) H55(0.5) C54(0.5) H54(0.5)
 C53(0.5) C52(0.5) H52(0.5) C51(0.5) H51(0.5) C50(0.5) C59(0.5) C56(0.5)
 C60(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C31(H31A,H31B), C37(H37A,H37B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15),
 C16(H16), C19(H19), C20(H20), C23(H23), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30), C33(H33), C34(H34), C36(H36), C046(H046), C48(H48), C46(H46),
 C45(H45), C43(H43), C42(H42), C49(H49), C40(H40), C39(H39), C55(H55), C54(H54),
  C52(H52), C51(H51)
;
_shelx_res_checksum              13263
_shelx_hkl_checksum              98117
_shelx_fab_checksum              83785