Controlled hierarchical self-assembly of networked coordination nanocapsules via the use of molecular chaperones
Hu, Xiangquan; Feng, Sisi; Du, Jialei; Shao, Li; Lang, Jinxin; Zhang, Chen; Kelley, Steven P.; Lin, Jian; Dalgarno, Scott J.; Atwood, David A.; Atwood, Jerry L.; Chemical Science 11 (2020) 12547–12552; doi:10.1039/D0SC05002D

data_1559726
_publ_section_title
;
 Controlled hierarchical self-assembly of networked coordination
 nanocapsules via the use of molecular chaperones
;
_journal_issue                   46
_journal_name_full               'Chemical Science'
_journal_page_first              12547
_journal_page_last               12552
_journal_paper_doi               10.1039/D0SC05002D
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         '0.25(C960 H768 Mn96 O560), 4(C2 H3 N)'
_chemical_formula_sum            'C248 H252 Mn24 N4 O140'
_chemical_formula_weight         6847.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   isomor
_audit_creation_date             2020-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-04 deposited with the CCDC.	2020-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.471(5)
_cell_length_b                   39.182(5)
_cell_length_c                   25.613(4)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      32.666
_cell_measurement_theta_min      4.378
_cell_volume                     37605(9)
_computing_cell_refinement       'Bruker Apex3 V.2017.3-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2017.3-0'
_computing_data_reduction        'Bruker Apex3 V.2017.3-0/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    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker VENTURE CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2472
_diffrn_reflns_av_unetI/netI     0.1175
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            164260
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        18.902
_diffrn_reflns_theta_max         18.902
_diffrn_reflns_theta_min         2.174
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.4982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             13952
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1843
_refine_ls_number_reflns         14844
_refine_ls_number_restraints     1961
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1834
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1244P)^2^+326.5034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7398
_reflns_number_total             14844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05002d2.cif
_cod_data_source_block           s1_sq
_cod_original_cell_volume        37604(9)
_cod_database_code               1559726
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37'-O15'
 1.54 with sigma of 0.04
 C30C-C31C
 1.54 with sigma of 0.04
 C31C-O13C
 1.4 with sigma of 0.04
 C16C-O7
 1.48 with sigma of 0.02
 C16C-O3
 1.48 with sigma of 0.02
 C36B-C37B = C37B-O15B
 1.54 with sigma of 0.04
 C35B-C37'
 2.54 with sigma of 0.04
 C30C-O13C
 2.54 with sigma of 0.06
 C35B-C37B = C36B-O15B
 2.54 with sigma of 0.04
3. 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
4. Others
 Sof(H36E)=Sof(H36F)=Sof(O15')=Sof(C37')=Sof(H37G)=Sof(H37H)=1-FVAR(1)
 Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(O15B)=FVAR(1)
 Fixed Sof: H16C(0.5) H16D(0.5) H16A(0.5) H16B(0.5) O3(0.5) O7(0.5)
 Fixed Uiso: C31C(0.25) C34A(0.25) O15C(0.25) O13C(0.25) C16C(0.25)
5.a Ternary CH refined with riding coordinates:
 C7A(H7A), C28B(H28B), C28A(H28A), C21A(H21A), C14B(H14B), C14A(H14A),
 C21B(H21B), C7B(H7B), C7C(H7C), C28C(H28C), C21C(H21C), C14C(H14C)
5.b Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C38B(H38A,H38B), C35A(H35A,H35B), C32B(H32A,H32B), C30A(H30A,
 H30B), C38A(H38C,H38D), C40B(H40A,H40B), C33B(H33A,H33B), C36A(H36A,H36B),
 C32A(H32C,H32D), C29B(H29C,H29D), C31A(H31A,H31B), C35B(H35C,H35D), C39B(H39A,
 H39B), C37A(H37A,H37B), C32C(H32E,H32F), C38C(H38E,H38F), C35C(H35E,H35F),
 C39A(H39C,H39D), C29C(H29E,H29F), C34B(H34A,H34B), C33A(H33C,H33D), C30B(H30C,
 H30D), C36B(H36C,H36D), C36B(H36E,H36F), C40A(H40C,H40D), C31B(H31C,H31D),
 C36C(H36G,H36H), C30C(H30E,H30F), C39C(H39E,H39F), C33C(H33E,H33F), C37B(H37C,
 H37D), C31C(H31E,H31F), C34A(H34C,H34D), C37C(H37E,H37F), C34C(H34E,H34F),
 C16C(H16C,H16D), C16C(H16A,H16B), C37'(H37G,H37H)
5.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C8A(H8A), C15A(H15A), C22B(H22B), C1B(H1B), C22A(H22A), C15C(H15C),
 C22C(H22C), C8B(H8B), C15B(H15B), C1C(H1C), C8C(H8C)
5.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              55856
_shelx_fab_checksum              41427
_olex2_submission_special_instructions 'No special instructions were received'