Endohedrally functionalised porous organic cages.
Burgun, Alexandre; Valente, Peter; Evans, Jack D.; Huang, David M.; Sumby, Christopher J.; Doonan, Christian J.; Chemical communications (Cambridge, England) 52 (2016) 8850–8853; doi:10.1039/c6cc04423a

data_7124758
_publ_section_title
;
 Endohedrally functionalised porous organic cages.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8850
_journal_page_last               8853
_journal_paper_doi               10.1039/c6cc04423a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C106 H56 N6 O2'
_chemical_formula_sum            'C106 H56 N6 O2'
_chemical_formula_weight         1445.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-21 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                102.93(3)
_cell_angle_beta                 101.11(3)
_cell_angle_gamma                112.55(3)
_cell_formula_units_Z            2
_cell_length_a                   16.792(3)
_cell_length_b                   19.978(4)
_cell_length_c                   23.171(5)
_cell_measurement_reflns_used    6228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      1.02
_cell_volume                     6654(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL_ifc (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44762
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        19.905
_diffrn_reflns_theta_max         19.905
_diffrn_reflns_theta_min         1.168
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    0.722
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The crystals have around 53% solvent accessible 
volume occupied with a possible mixture of 
toluene/hexane. This was not added
to the formula.
;
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         11599
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.442
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.1241
_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          0.3369
_refine_ls_wR_factor_ref         0.3559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7096
_reflns_number_total             11599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04423a2.cif
_cod_data_source_block           C1-N6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6654(3)
_cod_database_code               7124758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64-C66
 -2.3 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3AA(H3AA), C4AA(H4AA), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C2AA(H2AA), C20(H20), C21(H21), C29(H29), C30(H30), C31(H31),
 C40(H40), C41(H41), C37(H37), C38(H38), C44(H44), C45(H45), C47(H47), C48(H48),
  C54(H54), C55(H55), C56(H56), C66(H66), C64(H64), C65(H65), C71(H71),
 C70(H70), C74(H74), C73(H73), C76(H76), C77(H77), C79(H79), C80(H80), C86(H86),
  C87(H87), C88(H88), C96(H96), C97(H97), C98(H98), C105(H105), C101(H101),
 C102(H102), C103(H103), C108(H108), C109(H109), C111(H111), C112(H112)
3.b Fitted hexagon refined as free rotating group:
 C40(C41,C36,C37,C38,C39), C63(N62,C61,C66,C64,C65), C71(C70,C69,C74,C73,C72),
 C105(C101,C106,C102,C103,C104), C108(C109,C110,C111,C112,C107)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C114(H11A,H11B,H11C)
;
_shelx_res_checksum              29217
_shelx_hkl_checksum              99670
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'