Construction of Polymeric Metal-Organic Nanocapsule Networks via Supramolecular Coordination-Driven Self-Assembly.
Shao, Li; Hua, Bin; Hu, Xiangquan; Stalla, David; Kelley, Steven P.; Atwood, Jerry L.; Journal of the American Chemical Society 142 (2020) 7270–7275; doi:10.1021/jacs.0c00640

data_4134686
_publ_section_title
;
 Construction of Polymeric Metal-Organic Nanocapsule Networks via
 Supramolecular Coordination-Driven Self-Assembly.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7270
_journal_page_last               7275
_journal_paper_doi               10.1021/jacs.0c00640
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '0.33(C864 H900 Mg72 O378), 6(C2 H5 O2)'
_chemical_formula_sum            'C300 H420 Mg24 O138'
_chemical_formula_weight         6817.77
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   34.417(3)
_cell_length_b                   34.417(3)
_cell_length_c                   26.544(2)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.30
_cell_volume                     27230(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1174
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            157796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         2.367
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       fragment
_exptl_crystal_F_000             10836
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12438
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1383P)^2^+123.9679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8058
_reflns_number_total             12438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00640_si_002.cif
_cod_data_source_block           s1_sq
_cod_depositor_comments
'Adding full bibliography for 4134686--4134687.cif.'
_cod_original_cell_volume        27230(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4134686
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9457(8)
 0.0543(8)
2. 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, All C(H,H,H,H,H) groups
3. Restrained distances
 O7S-H7S = O1S-H1S
 0.92 with sigma of 0.02
 O2S-H2S
 0.92 with sigma of 0.02
4. Others
 Fixed Sof: H1SA(0.5) H1SB(0.5) H1SC(0.5) H1SD(0.5) H4SA(0.5) H4SB(0.5)
 H4SC(0.5) H4SD(0.5) H36A(0.5) H36B(0.5) H36C(0.5) H36D(0.5) O5S(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) O5S'(0.5) C2S'(0.5) H2SC(0.5) H2SD(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) H37C(0.5) C37'(0.5) H37D(0.5) H37E(0.5) H37F(0.5) C7S(0.6) C8S(0.6)
 C7S'(0.4) C8S'(0.4)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C7(H7A), C14(H14), C21(H21)
5.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C32(H32A,H32B), C29(H29A,H29B), C35(H35A,H35B), C33(H33A,
 H33B), C3S(H3SA,H3SB), C1S(H1SA,H1SB), C1S(H1SC,H1SD), C39(H39A,H39B),
 C4S(H4SA,H4SB), C4S(H4SC,H4SD), C30(H30A,H30B), C36(H36A,H36B), C36(H36C,H36D),
  C5S(H5SA,H5SB), C6S(H6SA,H6SB), C2S(H2SA,H2SB), C2S'(H2SC,H2SD)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C20(H20), C13(H13), C27(H27)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C31(H31A,H31B,H31C), C37(H37A,H37B,
 H37C), C37'(H37D,H37E,H37F)
;
_shelx_res_checksum              38957
_shelx_hkl_checksum              75278
_shelx_fab_checksum              66278
_olex2_submission_special_instructions 'No special instructions were received'