Guest control of structure in porous organic cages
Marc A. Little; Samantha Y. Chong; Marc Schmidtmann; Tom Hasell; Andrew I. Cooper; Chem.Commun. 50 (2014) 9465–; doi:10.1039/C4cc04158E

data_7115472
_publ_section_title
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 Guest control of structure in porous organic cages
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_journal_name_full               Chem.Commun.
_journal_page_first              9465
_journal_paper_doi               10.1039/C4cc04158E
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(H2 O), C66 H72 N12, 3(C8 H10)'
_chemical_formula_sum            'C90 H106 N12 O2'
_chemical_formula_weight         1387.87
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7488(15)
_cell_length_b                   19.2538(19)
_cell_length_c                   25.342(3)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.622
_cell_measurement_theta_min      2.263
_cell_volume                     8172.2(15)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            134283
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1250 before and 0.0745 after correction.
The Ratio of minimum to maximum transmission is 0.6215.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         13923
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+5.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                12428
_reflns_number_total             13923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04158e2.cif
_cod_data_source_block           CC4_Para_Xylene_Solvate_100K
_cod_original_cell_volume        8172.1(14)
_cod_database_code               7115472
_olex2_refinement_description
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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. Shared sites
{C83A, C83B}
{C84A, C84B}
{C86A, C86B}
{C87A, C87B}
{C85A, C85B}
{C88A, C88B}
3. Restrained distances
 C91-C84A = C89-C83A = C92-C87A = C86A-C90
 1.5 with sigma of 0.02
 C84A-C89 \\sim C88A-C89 \\sim C83A-C91 \\sim C85A-C91 \\sim C88A-C92 \\sim
C86A-C92 \\sim C85A-C90 ~
 C87A-C90
 with sigma of 0.02
4. Restrained planarity
 C91, C87A, C88A, C86A, C92, C83A, C85A, C90, C84A, C89
 with sigma of 0.001
5. Rigid bond restraints
 C81, C75, C76, C80, C77, C79, C78, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
Uiso(C83A) = Uiso(C83B)
Uiso(C87A) = Uiso(C87B)
Uiso(C86A) = Uiso(C86B)
Uiso(C84A) = Uiso(C84B)
Uiso(C88A) = Uiso(C88B)
Uiso(C85A) = Uiso(C85B)
7. Others
 Fixed Sof: C87A(0.5) C88A(0.5) H88A(0.5) C83A(0.5) H83A(0.5) C84A(0.5)
 C85A(0.5) H85A(0.5) C86A(0.5) H86A(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5)
 C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5) C91(0.5) H91A(0.5) H91B(0.5) H91C(0.5)
 C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C83B(0.5) C84B(0.5) H84B(0.5) C86B(0.5)
 C87B(0.5) H87B(0.5) C85B(0.5) H85B(0.5) C88B(0.5) H88B(0.5)
8.a Ternary CH refined with riding coordinates:
 C37(H37), C41(H41), C42(H42), C46(H46), C47(H47), C51(H51), C52(H52),
 C56(H56), C57(H57), C58(H58), C62(H62), C66(H66)
8.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C59(H59A,H59B), C60(H60A,H60B),
  C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
8.c Me refined with riding coordinates:
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C)
8.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C68(H68), C69(H69), C71(H71), C72(H72), C76(H76), C77(H77), C79(H79), C80(H80),
  C88A(H88A), C83A(H83A), C85A(H85A), C86A(H86A), C84B(H84B), C87B(H87B),
 C85B(H85B), C88B(H88B)
8.e Fitted hexagon refined as free rotating group:
 C87A(C88A,C83A,C84A,C85A,C86A)
8.f Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C)
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