Nanocapsules of unprecedented internal volume seamed by calcium ions.
Sikligar, Kanishka; Kelley, Steven P.; Wagle, Durgesh V.; Ishtaweera, Piyuni; Baker, Gary A.; Atwood, Jerry L.; Chemical science 14 (2023) 9063–9067; doi:10.1039/d3sc01629c

data_1569409
_publ_section_title
;
 Nanocapsules of unprecedented internal volume seamed by calcium ions.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              9063
_journal_page_last               9067
_journal_paper_doi               10.1039/d3sc01629c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C534 H534 Ca38 N24 Na24 O290'
_chemical_formula_sum            'C534 H732 Ca38 N24 Na24 O290'
_chemical_formula_weight         14202.19
_chemical_properties_physical    Air-sensitive,Deliquescent
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   calc
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2023-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   36.2373(12)
_cell_length_b                   36.2373(12)
_cell_length_c                   36.2373(12)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      42.90
_cell_measurement_theta_min      2.44
_cell_volume                     47585(3)
_computing_cell_refinement       'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2018.1-0'
_computing_data_reduction        'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            198100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.563
_diffrn_reflns_theta_max         44.563
_diffrn_reflns_theta_min         1.724
_diffrn_source                   'Incoatec IMuS microfocus Cu tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.512
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.5738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_description       Block
_exptl_crystal_F_000             14896
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         1837
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      2.081
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.1136
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3689
_refine_ls_wR_factor_ref         0.4261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1512
_reflns_number_total             1837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01629c2.cif
_cod_data_source_block           s1_sq
_cod_depositor_comments
'Adding full bibliography for 1569408--1569409.cif.'
_cod_original_cell_volume        47585(5)
_cod_database_code               1569409
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C7 \\sim C6-C7 \\sim C9-C6
 with sigma of 0.02
 C5-C6 \\sim C5-C4
 with sigma of 0.02
 C1-C2 \\sim C4-C1 \\sim C3-C4 \\sim C6-C7 \\sim C8-C7 \\sim C9-C6
 with sigma of 0.02
 O5-C12 \\sim O6-C12
 with sigma of 0.02
3. Restrained planarity
 Ca1, O10, O10_$8, Ca1_$9
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 O10(0.5) O7(0.25)
6.a Everything fixed:
 H12, H13
6.b Ternary CH refined with riding coordinates:
 C5(H5)
6.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
6.d Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
6.e Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C14(H14)
6.f Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              68690
_shelx_hkl_checksum              58219
_shelx_fab_checksum              37896
_olex2_submission_special_instructions 'No special instructions were received'