Catenation and encapsulation induce distinct reconstitutions within a dynamic library of mixed-ligand Zn4L6cages
Black, Samuel P.; Wood, Daniel M.; Schwarz, Felix B.; Ronson, Tanya K.; Holstein, Julian J.; Stefankiewicz, Artur R.; Schalley, Christoph A.; Sanders, Jeremy. K. M.; Nitschke, Jonathan R.; Chem. Sci. 7 (2016) 2614–; doi:10.1039/C5SC04906G

data_1542311
_publ_section_title
;
 Catenation and encapsulation induce distinct reconstitutions within a
 dynamic library of mixed-ligand Zn4L6cages
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2614
_journal_paper_doi               10.1039/C5SC04906G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C45 H50 N6 O Zn, 0.5(C H4 O)'
_chemical_formula_sum            'C45.5 H52.5 N6 O1.5 Zn'
_chemical_formula_weight         772.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-27 deposited with the CCDC.
2016-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.127(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3889(4)
_cell_length_b                   21.3112(10)
_cell_length_c                   11.1950(6)
_cell_measurement_reflns_used    6993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.985
_cell_measurement_theta_min      5.065
_cell_volume                     1998.43(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        'Bruker Apex II'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26343
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.572
_diffrn_reflns_theta_min         1.766
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       needle
_exptl_crystal_F_000             819
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8316
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1090P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                6057
_reflns_number_total             8316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04906g2.cif
_cod_data_source_block           dmw
_cod_depositor_comments
'Adding full bibliography for 1542311--1542313.cif.'
_cod_original_formula_sum        'C45.50 H52.50 N6 O1.50 Zn'
_cod_database_code               1542311
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.999
_shelxl_version_number           2013-2
_shelx_res_checksum              272