Concentration dependent supramolecular interconversions of triptycene-based cubic, prismatic, and tetrahedral structures.
Chakraborty, Sourav; Endres, Kevin J.; Bera, Ranajit; Wojtas, Lukasz; Moorefield, Charles N.; Saunders, Mary Jane; Das, Neeladri; Wesdemiotis, Chrys; Newkome, George R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14189–14194; doi:10.1039/c7dt04571a

data_7702167
_publ_section_title
;
 Concentration dependent supramolecular interconversions of
 triptycene-based cubic, prismatic, and tetrahedral structures.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14189
_journal_page_last               14194
_journal_paper_doi               10.1039/c7dt04571a
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C520 H328 N72 Zn12'
_chemical_formula_sum            'C520 H328 N72 Zn12'
_chemical_formula_weight         8368.96
_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_Hall           'F -4a 2 3'
_space_group_name_H-M_alt        'F -4 3 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-27 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   60.721(8)
_cell_length_b                   60.721(8)
_cell_length_c                   60.721(8)
_cell_measurement_reflns_used    9201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      8.72
_cell_measurement_theta_min      2.25
_cell_volume                     223881(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_wavelength     0.44281
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            414715
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        10.631
_diffrn_reflns_theta_max         10.631
_diffrn_reflns_theta_min         0.836
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.8879.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.497
_exptl_crystal_description       cube
_exptl_crystal_F_000             34496
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.461(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5665
_refine_ls_number_restraints     1186
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0996
_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^)+(0.1968P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2558
_refine_ls_wR_factor_ref         0.2567
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5534
_reflns_number_total             5665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04571a2.cif
_cod_data_source_block           4
_cod_original_cell_volume        223885(90)
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               7702167
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.996
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8-C7 = C3-C14 = C5-C20 = C38-C33 = C44-C37 = C50-C35
 1.49 with sigma of 0.02
 C41-C43 = C40-C38 = C33-C35 = N32-C36 = N45-C49 = C46-C48 = C51-C53 = C50-C54
 2.38 with sigma of 0.02
 C42-C40 = C41-N39 = C34-N32 = C33-C37 = C44-C46 = N45-C47 = C51-C55 = C50-C52
 2.38 with sigma of 0.02
 C42-C38 = C43-N39 = C34-C36 = C35-C37 = C44-C48 = C49-C47 = C52-C54 = C53-C55
 2.38 with sigma of 0.02
 C56-C54 = C57-C53 = C26-C24 = C27-C23
 1.5 with sigma of 0.02
 C17-C16 = C18-C17 = C19-C18 = C19-C14 = C4-C3 = C5-C4 = C6-C5 = C7-C6 = C8-
 C13 = C13-C12 = C12-C11 = C11-C10 = C41-C40 = C42-C41 = C43-C42 = C43-C38 =
 C34-C33 = C35-C34 = C36-C35 = C37-C36 = C49-C44 = C49-C48 = C48-C47 = C47-C46 =
  C51-C50 = C52-C51 = C53-C52 = C54-C53 = C55-C54 = C55-C50 = C21-C20 = C22-C21
 = C23-C22 = C24-C23 = C25-C24 = C25-C20
 1.39 with sigma of 0.02
 N15-C16 = N15-C14 = N2-C3 = N2-C7 = N9-C8 = N9-C10 = N39-C40 = N39-C38 = N32-
 C33 = N32-C37 = N45-C44 = N45-C46
 1.34 with sigma of 0.02
 C19-C17 = C14-C16 = C5-C3 = C6-N2 = C13-N9 = C12-C10 = C24-C20 = C23-C21
 2.38 with sigma of 0.02
 C18-C14 = C19-N15 = C4-C6 = C5-C7 = C25-C23 = C24-C22 = C8-C12 = C13-C11
 2.38 with sigma of 0.02
 C18-C16 = C17-N15 = C4-N2 = C3-C7 = C25-C21 = C20-C22 = C8-C10 = N9-C11
 2.38 with sigma of 0.02
 C8-C11 = N9-C12 = C13-C10 = C7-C4 = C6-C3 = C5-N2 = C22-C25 = C23-C20 = C24-
 C21 = C14-C17 = C19-C16 = C18-N15 = N39-C42 = C41-C38 = C40-C43 = N32-C35 =
 C33-C36 = C34-C37 = N45-C48 = C44-C47 = C49-C46 = C50-C53 = C55-C52 = C54-C51
 2.74 with sigma of 0.04
3. Restrained planarity
 C20, C21, C22, C23, C24, C25
 with sigma of 0.01
 C8, N9, C10, C11, C12, C13
 with sigma of 0.01
 C44, N45, C46, C47, C48, C49
 with sigma of 0.01
 N32, C33, C34, C35, C36, C37
 with sigma of 0.01
 C38, N39, C40, C41, C42, C43
 with sigma of 0.01
 C50, C51, C52, C53, C54, C55
 with sigma of 0.01
 N2, C3, C4, C5, C6, C7
 with sigma of 0.01
 C14, N15, C16, C17, C18, C19
 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Ternary CH refined with riding coordinates:
 C26(H26), C27(H27), C56(H56), C57(H57)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C34(H34), C36(H36), C40(H40),
  C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49),
 C51(H51), C52(H52), C55(H55)
;
_shelx_res_checksum              66546