Refolding Foldamers: Triazene-Arylene Oligomers That Change Shape with Chemical Stimuli
Simin Liu; Peter Y. Zavalij; Yiu-Fai Lam; Lyle Isaacs; Journal of the American Chemical Society 129 (2007) 11232–11241; doi:10.1021/ja073320s

data_4109906
_publ_section_title
;
 Refolding Foldamers: Triazene-Arylene Oligomers That Change Shape with
 Chemical Stimuli
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11232
_journal_page_last               11241
_journal_paper_doi               10.1021/ja073320s
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H60 N40 O20, C30 H30 N12 O2, I2'
_chemical_formula_sum            'C90 H189 I2 N52 O71.5'
_chemical_formula_weight         3397.73
_chemical_name_common            'CB10 melanime'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.756(3)
_cell_length_b                   14.2653(13)
_cell_length_c                   31.740(3)
_cell_measurement_reflns_used    7283
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      2.3
_cell_volume                     13926(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      606
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'cactus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0031965
_diffrn_orient_matrix_UB_12      -0.0697371
_diffrn_orient_matrix_UB_13      0.0010905
_diffrn_orient_matrix_UB_21      0.0319184
_diffrn_orient_matrix_UB_22      -0.0062438
_diffrn_orient_matrix_UB_23      0.0053491
_diffrn_orient_matrix_UB_31      -0.0053521
_diffrn_orient_matrix_UB_32      0.0035541
_diffrn_orient_matrix_UB_33      0.0310241
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26743
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.33
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             7084
_exptl_crystal_id
'Isaacs CB10.(NH2-Ph-NH-C3N3O-NH-)2-C10H6 H2O, KI, CF3COOH'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Total (Fo-Fc)map Electron Count in  Unit Cell =  1980

VOID-Fo-Fc-Map:    Rho(min) =     -0.39, Rho(max) =      6.80, RhoCutOff =  0.00
PeaksCloseToAtoms: Rho(min) =     -0.52, Rho(max) =      1.02, RhoCutOff =  0.50

:: Fo-scale =0.697149E+00 - SinT/L-Min = 0.20 for Fo/Fc-Scaling

:: Cycle = 23, R(F) = 0.08, Nref(Hemi) = 34511, R(F > 4SIGF) = 0.05 Nref = 25672
;
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.417(16)
_refine_ls_extinction_coef       0.00017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1583
_refine_ls_number_reflns         15835
_refine_ls_number_restraints     1022
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0532
_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^)+(0.02P)^2^+23.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.737
_reflns_number_gt                12203
_reflns_number_total             15835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073320ssi20070510_095943.cif
_cod_data_source_block           1376
_cod_depositor_comments
;
 Removing the _chemical_name_systematic data item since it contains the
 common chemical name which is already recorded using the _chemical_name_common
 data item.

 Antanas Vaitkus,
 2018-10-12
;
_cod_original_formula_sum        'C90 H189 I2 N52 O71.50'
_cod_database_code               4109906
_diffrn_measurement_total_frames-ccd 606
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.939
_diffrn_measurement_frame_time-ccd 38
_diffrn_measurement_total_time-ccd 7.60
_diffrn_measurement_frame_size-ccd 512