Linear Supramolecular Polymers Driven by Anion-Anion Dimerization of Difunctional Phosphonate Monomers Inside Cyanostar Macrocycles.
Zhao, Wei; Qiao, Bo; Tropp, Joshua; Pink, Maren; Azoulay, Jason D.; Flood, Amar H.; Journal of the American Chemical Society 141 (2019) 4980–4989; doi:10.1021/jacs.9b00248

data_4129026
_publ_section_title
;
 Linear Supramolecular Polymers Driven by Anion-Anion Dimerization of
 Difunctional Phosphonate Monomers Inside Cyanostar Macrocycles.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4980
_journal_page_last               4989
_journal_paper_doi               10.1021/jacs.9b00248
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C95.44 H136.52 Cl0.37 N6 O5.82 P'
_chemical_formula_weight         1505.08
_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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                63.1338(18)
_cell_angle_beta                 76.4813(19)
_cell_angle_gamma                68.8934(19)
_cell_formula_units_Z            2
_cell_length_a                   16.1688(6)
_cell_length_b                   18.0527(8)
_cell_length_c                   18.8483(8)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.25
_cell_volume                     4561.9(3)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.980
_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       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57111
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.847
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2014'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         17293
_refine_ls_number_restraints     1752
_refine_ls_restrained_S_all      1.990
_refine_ls_R_factor_all          0.1754
_refine_ls_R_factor_gt           0.1139
_refine_ls_shift/su_max          0.013
_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          0.3151
_refine_ls_wR_factor_ref         0.3375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9468
_reflns_number_total             17293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00248_si_002.cif
_cod_data_source_block           17155
_cod_database_code               4129026
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2014-3
_shelx_res_checksum              19042
_shelx_hkl_checksum              60999