Kinetically controlled fast crystallization of M12L8 poly-[n]-catenanes using the 2,4,6-tris(4-pyridyl)benzene ligand and ZnCl2 in aromatic environment.
Torresi, Stefano; Famulari, Antonino; Marti-Rujas, Javier; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03319

data_4134928
_publ_section_title
;
 Kinetically controlled fast crystallization of M12L8 poly-[n]-catenanes
 using the 2,4,6-tris(4-pyridyl)benzene ligand and ZnCl2 in aromatic
 environment.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03319
_journal_year                    2020
_chemical_formula_sum            'C21 H15 N3'
_chemical_formula_weight         309.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1389(2)
_cell_length_b                   10.96400(10)
_cell_length_c                   7.08510(10)
_cell_measurement_reflns_used    10084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      3.67280677933
_cell_measurement_theta_min      25.7336281823
_cell_volume                     1486.73(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD Pilatus 6M-Dectris'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.72931
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            15952
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.727
_diffrn_reflns_theta_max         25.727
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'Alba-CELLS, Barcelona, Catalonia, Spain'
_exptl_absorpt_coefficient_mu    0.083
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 608 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1363
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.4053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1342
_reflns_number_total             1363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03319_si_002.cif
_cod_data_source_block           TPB@ALBA_Cells_Barcelona2019
_cod_database_code               4134928
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              35425
_shelx_hkl_checksum              94119