Template-directed self-assembly of dynamic covalent capsules with polar interiors
Galan, Albano; Escudero, Eduardo Carmelo; Ballester, Pablo; Chem. Sci.  (2017) –; doi:10.1039/C7SC03731G

data_1547369
_publ_section_title
;
 Template-directed self-assembly of dynamic covalent capsules with polar
 interiors
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03731G
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C170 H155.5 N18 O3'
_chemical_formula_weight         2498.61
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_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-2014/7
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.046(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6872(16)
_cell_length_b                   22.135(3)
_cell_length_c                   24.856(3)
_cell_measurement_reflns_used    1867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.26
_cell_measurement_theta_min      2.30
_cell_volume                     7511.8(16)
_computing_cell_refinement       'Bruker APEX2 v2014.9-0'
_computing_data_collection       'Bruker APEX2 v2014.9-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_unetI/netI     0.2463
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28794
_diffrn_reflns_point_group_measured_fraction_full 0.771
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        23.248
_diffrn_reflns_theta_max         23.248
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2651
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 1448 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1813
_refine_ls_number_reflns         16617
_refine_ls_number_restraints     1623
_refine_ls_restrained_S_all      1.898
_refine_ls_R_factor_all          0.2986
_refine_ls_R_factor_gt           0.1397
_refine_ls_shift/su_max          0.026
_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          0.2872
_refine_ls_wR_factor_ref         0.3541
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.589
_reflns_Friedel_fraction_max     0.589
_reflns_number_gt                6197
_reflns_number_total             16617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03731g2.cif
_cod_data_source_block           mo_AGextB1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        7512.0(15)
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C170 H155.50 N18 O3'
_cod_database_code               1547369
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              34604