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_4122287
_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, C18 H12, 6(F6 P), 10(C2 H3 N)'
_chemical_formula_sum            'C104 H96 F36 N16 P6'
_chemical_formula_weight         2439.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2013-06-10
_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                   18.1424(6)
_cell_length_b                   28.4624(9)
_cell_length_c                   21.3281(6)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.41
_cell_measurement_theta_min      3.11
_cell_volume                     11013.3(6)
_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
;
SHELXD, 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 0.970
_diffrn_measured_fraction_theta_max 0.980
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45546
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.151
_diffrn_reflns_theta_min         2.888
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0468 before and 0.0389 after correction.
The Ratio of minimum to maximum transmission is 0.8648.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0899P)^2^+7.1774P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                9615
_reflns_number_total             9812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_002.cif
_cod_data_source_block           n2802a
_cod_database_code               4122287
_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-C41 \\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 C50-C45 \\sim C51-C50 \\sim C52-C51 \\sim 
 C53-C52 \\sim C54-C53 \\sim C54-
 C49 \\sim C55-C54 \\sim C56-C55 \\sim C57-C56 \\sim C58-C57 \\sim C58-C53
 with sigma of 0.02
 C41-C43 \\sim C42-C44 \\sim C45-C47 \\sim C46-C48 \\sim C49-C51 \\sim C50-C52
 \\sim C53-C55 \\sim C54-C58
 \\sim C58-C56 \\sim C57-C53
 with sigma of 0.02
 C41-C44 \\sim C42-C45 \\sim C43-C46 \\sim C47-C50 \\sim C49-C52 \\sim C51-C54 
 \\sim C53-C56 \\sim C55-C58
 \\sim C48-C45 \\sim C57-C54
 with sigma of 0.02
3. Rigid bond restraints
 C51, C57, C58, C56, C53, C55, C54, C52, C49, C48, C50, C47, C45, C46, C44,
 C41, C43, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(N7S)=Sof(C13S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(N6S)=Sof(C11S)=Sof(C12S)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H13A(0.5) H13B(0.5) H18A(0.5) H18B(0.5) C41(0.5) H41(0.5) C42(0.5)
 H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) C46(0.5) C47(0.5)
 H47(0.5) C48(0.5) H48(0.5) C49(0.5) C50(0.5) C51(0.5) H51(0.5) C52(0.5)
 H52(0.5) C53(0.5) C54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5) C57(0.5)
 H57(0.5) C58(0.5) H58(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5) H4SA(0.5) H4SB(0.5)
 H4SC(0.5) N3S(0.5) C5S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) H8SB(0.5)
 H8SC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C31(H31A,H31B), C38(H38A,H38B)
5.b Me refined with riding coordinates:
 C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,H8SC)
5.c 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), C37(H37), C41(H41), C42(H42),
 C43(H43), C44(H44), C47(H47), C48(H48), C51(H51), C52(H52), C55(H55), C56(H56),
  C57(H57), C58(H58)
5.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C10S(H10A,H10B,H10C), C12S(H12A,
 H12B,H12C), C14S(H14A,H14B,H14C), C18S(H18C,H18D,H18E)
;
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.614
_shelxl_version_number           2012-9