Formation of ring-in-ring complexes between crown ethers and rigid TVBox(8+).
Sun, Junling; Frasconi, Marco; Liu, Zhichang; Barnes, Jonathan C.; Wang, Yuping; Chen, Dongyang; Stern, Charlotte L.; Fraser Stoddart, J.; Chemical communications (Cambridge, England) 51 (2015) 1432–1435; doi:10.1039/c4cc08053j

data_7116224
_publ_section_title
;
 Formation of ring-in-ring complexes between crown ethers and rigid
 TVBox(8+).
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1432
_journal_page_last               1435
_journal_paper_doi               10.1039/c4cc08053j
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C68 H56 N8, 4(C6 H5 Cl), 8(F6 P), 8(C2 H3 N)'
_chemical_formula_sum            'C108 H100 Cl4 F48 N16 P8'
_chemical_formula_weight         2923.59
_chemical_name_systematic        TVBox-PhCl
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-08-28 deposited with the CCDC.
2014-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9615(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8603(4)
_cell_length_b                   16.2006(5)
_cell_length_c                   27.9776(8)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.062
_cell_measurement_theta_min      4.261
_cell_volume                     6122.2(3)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35631
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.057
_diffrn_reflns_theta_min         4.238
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.020
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0520 before and 0.0365 after correction.
The Ratio of minimum to maximum transmission is 0.8088.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       needle
_exptl_crystal_F_000             2960
_exptl_crystal_recrystallization_method
'slow vapor diffusion of diisopropyl ether into the sample solution in ACN'
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0752P)^2^+10.6839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9480
_reflns_number_total             10353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08053j2.cif
_cod_data_source_block           n3299
_cod_depositor_comments
'Adding full bibliography for 7116222--7116224.cif.'
_cod_database_code               7116224
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.432
_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
 F17A, F13A, F15, F14, F15A, F13, F17, F14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F17A \\sim F13A \\sim F15 \\sim F14 \\sim F15A \\sim F13 \\sim F17 \\sim F14A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F17A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F17)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46)
5.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C)
;
_shelx_res_checksum              67535