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_1559725
_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         'C250 H140 Mn24 N2 O130'
_chemical_formula_sum            'C250 H258 Mn24 N2 O130'
_chemical_formula_weight         6689.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-18
_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                 95.026(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.3705(17)
_cell_length_b                   32.550(2)
_cell_length_c                   22.5838(17)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      22.91
_cell_measurement_theta_min      2.19
_cell_volume                     16381(2)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            223225
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.386
_diffrn_reflns_theta_max         23.386
_diffrn_reflns_theta_min         1.229
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6582
_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    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             6824
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.443
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.678
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1581
_refine_ls_number_reflns         23785
_refine_ls_number_restraints     1534
_refine_ls_restrained_S_all      1.661
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.1318
_refine_ls_shift/su_max          0.001
_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          0.3923
_refine_ls_wR_factor_ref         0.4373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14496
_reflns_number_total             23785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05002d2.cif
_cod_data_source_block           s1_a_sq
_cod_database_code               1559725
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.800
_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
2. Restrained distances
 C34-C33 = C33-C32
 1.54 with sigma of 0.02
 C73-C72 = C74-C73 = C76-C75 = C77-C76
 1.54 with sigma of 0.02
 C30-C29 = C30-C31
 1.54 with sigma of 0.02
 C31-O37
 1.48 with sigma of 0.02
 C80-C79
 1.54 with sigma of 0.02
 O44-C80
 1.48 with sigma of 0.02
 C73-C72 = C74-C73
 1.54 with sigma of 0.02
 C73-C74' = C74-C73 = C73-C72
 1.54 with sigma of 0.02
 O42-C74
 1.48 with sigma of 0.02
 O42'-C74'
 1.48 with sigma of 0.02
 C79-C80'
 1.54 with sigma of 0.02
 O46'-C114
 1.48 with sigma of 0.02
 C114-C113
 1.54 with sigma of 0.02
 C79-C78 = C79'-C78 = C80-C79 = C80'-C79'
 1.54 with sigma of 0.02
 O44-C80 = O44'-C80'
 1.48 with sigma of 0.02
 C3'P-C4'P = C4'P-C5'P
 1.54 with sigma of 0.02
 C115-C116
 1.54 with sigma of 0.02
 C2P-C3'P
 1.54 with sigma of 0.02
 N1P-C5'P
 1.48 with sigma of 0.02
 O46'-C113
 -2.3 with sigma of 0.02
 C118-C108 = C119-C118 = C120-C119
 1.54 with sigma of 0.02
 O48-C120
 1.48 with sigma of 0.02
 O46-C114
 1.48 with sigma of 0.02
 C113-O46
 -2.3 with sigma of 0.02
 C34-C33
 -2.3 with sigma of 0.02
 C34-C33 = C34'-C33
 1.54 with sigma of 0.02
 O38-C34' = O38-C34
 1.48 with sigma of 0.02
 O38-C33
 -2.3 with sigma of 0.02
 O43-C77
 1.48 with sigma of 0.02
 O47-C117
 1.48 with sigma of 0.02
 C117-C116 = C116-C115 = C115-C101
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C80' \\sim C80: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
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
 Uiso(C2P)=Uiso(C3P)=Uiso(C4P)=Uiso(C5P)=Uiso(C4'P)=Uiso(C3'P)=Uiso(C5'P)=
 FVAR(1)
 Fixed Sof: H11C(0.5) H11D(0.5) H11E(0.5) H11F(0.5) H78A(0.5) H78B(0.5)
 H78C(0.5) H78D(0.5) C79(0.5) H79A(0.5) H79B(0.5) C34(0.5) C74(0.5) O44(0.5)
 C80(0.5) H80A(0.5) H80B(0.5) O42(0.5) O42'(0.5) C74'(0.5) C80'(0.5) H80C(0.5)
 H80D(0.5) C79'(0.5) H79C(0.5) H79D(0.5) O44'(0.5) C3P(0.5) C4P(0.5) C5P(0.5)
 C4'P(0.5) C3'P(0.5) C5'P(0.5) C119(0.5) O48(0.5) C120(0.5) O48'(0.5) C19'(0.5)
 C20'(0.5) O46(0.5) C34'(0.5) O43(0.5)
6.a Free rotating group:
 C1P(C2P,O2P,O1P,C3P,N1P,C4P,C5P)
6.b Ternary CH refined with riding coordinates:
 C87(H87), C14(H14), C28(H28), C21(H21), C7(H7), C47(H47), C94(H94),
 C108(H108), C61(H61), C101(H101), C68(H68), C54(H54)
6.c Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C38(H38A,H38B), C69(H69A,H69B), C109(H10A,H10B), C32(H32A,
 H32B), C70(H70A,H70B), C29(H29A,H29B), C112(H11A,H11B), C118(H11C,H11D),
 C118(H11E,H11F), C110(H11G,H11H), C111(H11I,H11J), C75(H75A,H75B), C78(H78A,
 H78B), C78(H78C,H78D), C71(H71A,H71B), C39(H39A,H39B), C115(H11K,H11L),
 C79(H79A,H79B), C76(H76A,H76B), C40(H40A,H40B), C36(H36A,H36B), C113(H11M,
 H11N), C72(H72A,H72B), C80(H80A,H80B), C80'(H80C,H80D), C79'(H79C,H79D)
6.d Aromatic/amide H refined with riding coordinates:
 C100(H100), C53(H53), C27(H27), C20(H20), C5(H5), C13(H13), C85(H85),
 C67(H67), C93(H93), C60(H60), C45(H45), C107(H107)
;
_shelx_res_checksum              73247
_shelx_fab_checksum              9751
_olex2_submission_special_instructions 'No special instructions were received'