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_4134687
_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         'C261 H253 Mg24 N2 O125, O, C4 H8 O3'
_chemical_formula_sum            'C265 H296 Mg24 N2 O129'
_chemical_formula_weight         6156.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.801(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.025(5)
_cell_length_b                   36.916(5)
_cell_length_c                   26.530(4)
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.23
_cell_volume                     36134(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    '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 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  0.0841
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            405391
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.347
_diffrn_reflns_theta_max         23.347
_diffrn_reflns_theta_min         2.165
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             12880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3781
_refine_ls_number_reflns         52201
_refine_ls_number_restraints     5148
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0890
_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^)+(0.1735P)^2^+82.6293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2539
_refine_ls_wR_factor_ref         0.2987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32597
_reflns_number_total             52201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00640_si_003.cif
_cod_data_source_block           s1_sq
_cod_depositor_comments
'Adding full bibliography for 4134686--4134687.cif.'
_cod_database_code               4134687
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.969
_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. 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
3.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C47(H47), C54(H54), C61(H61), C68(H68),
 C87(H87), C94(H94), C101(H101), C108(H108), C127(H127), C134(H134), C141(H141),
  C148(H148), C167(H167), C174(H174), C181(H181), C188(H188), C207(H207),
 C214(H214), C221(H221), C228(H228)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,
 H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C69(H69A,H69B),
 C70(H70A,H70B), C72(H72A,H72B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B),
  C78(H78A,H78B), C79(H79A,H79B), C109(H10A,H10B), C110(H11A,H11B), C112(H11F,
 H11G), C113(H11H,H11I), C115(H11M,H11N), C116(H11O,H11P), C118(H11T,H11U),
 C119(H11V,H11W), C149(H14A,H14B), C150(H15A,H15B), C152(H15F,H15G), C153(H15H,
 H15I), C155(H15M,H15N), C156(H15O,H15P), C158(H15T,H15U), C159(H15V,H15W),
 C189(H18A,H18B), C190(H19A,H19B), C192(H19F,H19G), C193(H19H,H19I), C195(H19M,
 H19N), C196(H19O,H19P), C198(H19T,H19U), C199(H19V,H19W), C229(H22A,H22B),
 C230(H23A,H23B), C232(H23F,H23G), C233(H23H,H23I), C235(H23M,H23N), C236(H23O,
 H23P), C238(H23T,H23U), C239(H23V,H23W), C241(H24D,H24E), C242(H24F,H24G),
 C243(H24H,H24I), C244(H24J,H24K), C245(H24L,H24M), C246(H24N,H24O), C247(H24P,
 H24Q), C248(H24R,H24S), C249(H24T,H24U), C250(H25A,H25B), C251(H25C,H25D),
 C252(H25E,H25F), C253(H25G,H25H), C254(H25I,H25J), C255(H25K,H25L), C256(H25M,
 H25N), C262(H26A,H26B), C263(H26C,H26D), C264(H26E,H26F), C265(H26G,H26H)
3.c Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C40(H40A,H40B,
 H40C), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C), C77(H77A,H77B,H77C), C80(H80A,
 H80B,H80C), C111(H11C,H11D,H11E), C114(H11J,H11K,H11L), C117(H11Q,H11R,H11S),
 C120(H12A,H12B,H12C), C151(H15C,H15D,H15E), C154(H15J,H15K,H15L), C157(H15Q,
 H15R,H15S), C160(H16A,H16B,H16C), C191(H19C,H19D,H19E), C194(H19J,H19K,H19L),
 C197(H19Q,H19R,H19S), C200(H20A,H20B,H20C), C231(H23C,H23D,H23E), C234(H23J,
 H23K,H23L), C237(H23Q,H23R,H23S), C240(H24A,H24B,H24C)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C13(H13), C20(H20), C27(H27), C45(H45), C53(H53), C60(H60), C67(H67),
 C85(H85), C93(H93), C99(H99), C107(H107), C125(H125), C133(H133), C140(H140),
 C147(H147), C165(H165), C173(H173), C180(H180), C187(H187), C205(H205),
 C213(H213), C220(H220), C227(H227), C257(H257), C258(H258), C259(H259),
 C260(H260), C261(H261)
;
_shelx_res_checksum              4088
_shelx_hkl_checksum              95718
_shelx_fab_checksum              3623
_olex2_submission_special_instructions 'No special instructions were received'