Tunable Adhesion from Stoichiometry-controlled and Sequence-defined Supramolecular Polymers Emerges Hierarchically from Cyanostar-stabilized Anion-anion Linkages.
Zhao, Wei; Tropp, Joshua; Qiao, Bo; Pink, Maren; Azoulay, Jason D.; Flood, Amar H.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12645

data_4134039
_publ_section_title
;
 Tunable Adhesion from Stoichiometry-controlled and Sequence-defined
 Supramolecular Polymers Emerges Hierarchically from Cyanostar-stabilized
 Anion-anion Linkages.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12645
_journal_year                    2020
_chemical_formula_moiety
'C65H65N5, 2 C16H36N, C6H6O8P2, 2(CH4O), 0.25(CH2Cl2), 0.25(H2O)'
_chemical_formula_sum            'C105.25 H152 Cl0.5 N7 O10.25 P2'
_chemical_formula_weight         1758.99
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                87.692(4)
_cell_angle_beta                 85.637(4)
_cell_angle_gamma                68.070(4)
_cell_formula_units_Z            4
_cell_length_a                   18.5691(13)
_cell_length_b                   19.7813(14)
_cell_length_c                   34.092(2)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.34
_cell_volume                     11582.0(14)
_computing_cell_refinement       'APEX II v2014.11-0 (Bruker, 2018)'
_computing_data_collection       'APEX II v2014.11-0 (Bruker, 2018)'
_computing_data_reduction        'APEX II v2014.11-0 (Bruker, 2018)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2018)'
_computing_publication_material  'SHELXTL (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
'0.50 degree frames measured for 180 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            107970
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.004
_diffrn_reflns_theta_min         1.821
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2018'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       block
_exptl_crystal_F_000             3812
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.484
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2684
_refine_ls_number_reflns         53318
_refine_ls_number_restraints     5443
_refine_ls_restrained_S_all      2.007
_refine_ls_R_factor_all          0.2372
_refine_ls_R_factor_gt           0.1466
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3744
_refine_ls_wR_factor_ref         0.4053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26007
_reflns_number_total             53318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12645_si_002.cif
_cod_data_source_block           17149
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        11581.9(14)
_cod_original_formula_sum        'C105.25 H152 Cl0.50 N7 O10.25 P2'
_cod_database_code               4134039
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              83626
_shelx_hkl_checksum              55638