Mechanically Interlocked Linkers inside Metal-Organic Frameworks: Effect of Ring Size on Rotational Dynamics.
Vukotic, V. Nicholas; O'Keefe, Christopher A; Zhu, Kelong; Harris, Kristopher J.; To, Christine; Schurko, Robert W.; Loeb, Stephen J.; Journal of the American Chemical Society  (2015) 150723135020006–; doi:10.1021/jacs.5b04674

data_4124189
_publ_section_title
;
 Mechanically Interlocked Linkers inside Metal-Organic Frameworks: Effect
 of Ring Size on Rotational Dynamics.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150723135020006
_journal_paper_doi               10.1021/jacs.5b04674
_journal_year                    2015
_chemical_formula_moiety         'C25 H29 N O8, C22 H36 O6'
_chemical_formula_sum            'C47 H65 N O14'
_chemical_formula_weight         868.00
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.2190(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8754(12)
_cell_length_b                   34.211(3)
_cell_length_c                   18.0716(15)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.172
_cell_measurement_theta_min      3.046
_cell_volume                     9322.9(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.06
_diffrn_measured_fraction_theta_full 0.718
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_laue_measured_fraction_full 0.718
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            151091
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.465
_diffrn_reflns_theta_min         2.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012)
wR2(int)was 0.0720 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8859.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1238
_refine_ls_number_reflns         12110
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.1113
_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^)+(0.0177P)^2^+39.4543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8559
_reflns_number_total             12110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04674_si_003.cif
_cod_data_source_block           mo_nv008_0m
_cod_original_cell_volume        9323.0(13)
_cod_database_code               4124189
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O109 \\sim O110 \\sim O111 \\sim O112 \\sim O113 \\sim O114 \\sim C126 \\sim
C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim
C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139 \\sim C140 \\sim
C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim C147: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O209 \\sim O210 \\sim O211 \\sim O212 \\sim O213 \\sim O214 \\sim C226 \\sim
C227 \\sim C228 \\sim C229 \\sim C230 \\sim C231 \\sim C232 \\sim C233 \\sim
C234 \\sim C235 \\sim C236 \\sim C237 \\sim C238 \\sim C239 \\sim C240 \\sim
C241 \\sim C242 \\sim C243 \\sim C244 \\sim C245 \\sim C246 \\sim C247: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C113 \\sim N101 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C104 \\sim
C105: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N201 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217 \\sim C218 \\sim
C219: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Sof(N201)=Sof(H201)=Sof(C213)=Sof(H21A)=Sof(H21B)=Sof(C214)=Sof(C215)=
 Sof(H215)=Sof(C216)=Sof(C217)=Sof(H217)=Sof(C218)=Sof(C219)=Sof(H219)=
 Sof(O209)=Sof(O210)=Sof(O211)=Sof(O212)=Sof(O213)=Sof(O214)=Sof(C226)=
 Sof(H22A)=Sof(H22B)=Sof(C227)=Sof(H22C)=Sof(H22D)=Sof(C228)=Sof(H22E)=
 Sof(H22F)=Sof(C229)=Sof(H22G)=Sof(H22H)=Sof(C230)=Sof(C231)=Sof(H231)=
 Sof(C232)=Sof(H232)=Sof(C233)=Sof(H233)=Sof(C234)=Sof(H234)=Sof(C235)=
 Sof(C236)=Sof(H23A)=Sof(H23B)=Sof(C237)=Sof(H23C)=Sof(H23D)=Sof(C238)=
 Sof(H23E)=Sof(H23F)=Sof(C239)=Sof(H23G)=Sof(H23H)=Sof(C240)=Sof(H24A)=
 Sof(H24B)=Sof(C241)=Sof(H24C)=Sof(H24D)=Sof(C242)=Sof(H24E)=Sof(H24F)=
 Sof(C243)=Sof(H24G)=Sof(H24H)=Sof(C244)=Sof(H24I)=Sof(H24J)=Sof(C245)=
 Sof(H24K)=Sof(H24L)=Sof(C246)=Sof(H24M)=Sof(H24N)=Sof(C247)=Sof(H24O)=
 Sof(H24P)=1-FVAR(1)
 Sof(C113)=Sof(H11F)=Sof(H11G)=Sof(N101)=Sof(H101)=Sof(C104)=Sof(C105)=
 Sof(H105)=Sof(C106)=Sof(C107)=Sof(H107)=Sof(C108)=Sof(C109)=Sof(H109)=
 Sof(O109)=Sof(O110)=Sof(O111)=Sof(O112)=Sof(O113)=Sof(O114)=Sof(C126)=
 Sof(H12K)=Sof(H12L)=Sof(C127)=Sof(H12M)=Sof(H12N)=Sof(C128)=Sof(H12O)=
 Sof(H12P)=Sof(C129)=Sof(H12Q)=Sof(H12R)=Sof(C130)=Sof(C131)=Sof(H131)=
 Sof(C132)=Sof(H132)=Sof(C133)=Sof(H133)=Sof(C134)=Sof(H134)=Sof(C135)=
 Sof(C136)=Sof(H13A)=Sof(H13B)=Sof(C137)=Sof(H13C)=Sof(H13D)=Sof(C138)=
 Sof(H13E)=Sof(H13F)=Sof(C139)=Sof(H13G)=Sof(H13H)=Sof(C140)=Sof(H14A)=
 Sof(H14B)=Sof(C141)=Sof(H14C)=Sof(H14D)=Sof(C142)=Sof(H14E)=Sof(H14F)=
 Sof(C143)=Sof(H14G)=Sof(H14H)=Sof(C144)=Sof(H14I)=Sof(H14J)=Sof(C145)=
 Sof(H14K)=Sof(H14L)=Sof(C146)=Sof(H14M)=Sof(H14N)=Sof(C147)=Sof(H14O)=
 Sof(H14P)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11H,H11I), C13(H13I,H13J), C21(H21C,H21D), C24(H24Q,H24R),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C102(H10D,H10E), C111(H11A,H11B), C121(H12A,
 H12B), C124(H12F,H12G), C113(H11F,H11G), C126(H12K,H12L), C127(H12M,H12N),
 C128(H12O,H12P), C129(H12Q,H12R), C136(H13A,H13B), C137(H13C,H13D), C138(H13E,
 H13F), C139(H13G,H13H), C140(H14A,H14B), C141(H14C,H14D), C142(H14E,H14F),
 C143(H14G,H14H), C144(H14I,H14J), C145(H14K,H14L), C146(H14M,H14N), C147(H14O,
 H14P), C213(H21A,H21B), C226(H22A,H22B), C227(H22C,H22D), C228(H22E,H22F),
 C229(H22G,H22H), C236(H23A,H23B), C237(H23C,H23D), C238(H23E,H23F), C239(H23G,
 H23H), C240(H24A,H24B), C241(H24C,H24D), C242(H24E,H24F), C243(H24G,H24H),
 C244(H24I,H24J), C245(H24K,H24L), C246(H24M,H24N), C247(H24O,H24P)
4.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C12(H12S,H12T,H12U), C22(H22I,H22J,H22K), C25(H25A,H25B,
 H25C), C101(H10A,H10B,H10C), C112(H11C,H11D,H11E), C122(H12C,H12D,H12E),
 C125(H12H,H12I,H12J)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C7(H7), C9(H9), C15(H15), C17(H17), C19(H19), C31(H31),
 C32(H32), C33(H33), C34(H34), C115(H115), C117(H117), C119(H119), N101(H101),
 C105(H105), C107(H107), C109(H109), C131(H131), C132(H132), C133(H133),
 C134(H134), N201(H201), C215(H215), C217(H217), C219(H219), C231(H231),
 C232(H232), C233(H233), C234(H234)
4.d Fitted hexagon refined as free rotating group:
 C214(C215,C216,C217,C218,C219), C230(C231,C232,C233,C234,C235)
;
_olex2_submission_special_instructions 'No special instructions were received'