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_4122288
_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, 0.5(C40 H24), 6(F6 P), C4 H6 N2'
_chemical_formula_sum            'C90 H72 F36 N8 P6'
_chemical_formula_weight         2135.37
_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             2013-08-02
_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                   18.0778(18)
_cell_length_b                   28.704(2)
_cell_length_c                   21.242(2)
_cell_measurement_reflns_used    5096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.77
_cell_measurement_theta_min      6.17
_cell_volume                     11022.6(17)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.972
_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  0.1152
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23404
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.12
_diffrn_reflns_theta_min         6.17
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1016 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.8312.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0819
_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^)+(0.1572P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2764
_reflns_number_total             4740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5041557_si_007.cif
_cod_data_source_block           n2925
_cod_original_cell_volume        11022.7(17)
_cod_database_code               4122288
_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. Rigid bond restraints
 C28, C30, C31, C32, C29, C39, C33, C36, C34, C27, C37, C35, C38, C26, C20,
 C23, C25, C21, C22, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C28 \\sim C30 \\sim C31 \\sim C32 \\sim C29 \\sim C39 \\sim C33 \\sim C36 \\sim C34 \\sim C27 \\sim C37 \\sim C35 \\sim C38 \\sim C26 \\sim C20 \\sim C23 \\sim C25 \\sim C21 \\sim C22 \\sim C24: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H3A(0.5) H3B(0.5) C20(0.25) H20(0.25) C21(0.25) H21(0.25)
 C22(0.25) H22(0.25) C23(0.25) C24(0.25) H24(0.25) C25(0.25) H25(0.25)
 C26(0.25) H26(0.25) C27(0.25) C28(0.25) C29(0.25) H29(0.25) C30(0.25)
 H30(0.25) C31(0.25) H31(0.25) C32(0.25) C33(0.25) H33(0.25) C34(0.25)
 H34(0.25) C35(0.25) H35(0.25) C36(0.25) C37(0.25) C38(0.25) C39(0.25)
 H41A(0.5) H41B(0.5) H41C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C16(H16A,H16B)
5.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), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
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_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 = 2542.6 Ang^3 [23.1%]
Total electron count / cell = 116.4
;
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.885
_shelx_hkl_checksum              81901
_shelx_res_checksum              48374
_shelxl_version_number           2012-9