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_4124190
_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, C16 H32 O6'
_chemical_formula_sum            'C41 H61 N O14'
_chemical_formula_weight         791.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.937(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5899(11)
_cell_length_b                   20.674(3)
_cell_length_c                   12.1902(15)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.08
_cell_measurement_theta_min      3.63
_cell_volume                     2159.7(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX II'
_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)'
_diffrn_ambient_temperature      150.21
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32210
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.403
_diffrn_reflns_theta_min         3.634
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0743 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8952.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 3008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.53(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7097
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1247P)^2^+1.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                6696
_reflns_number_total             7097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04674_si_002.cif
_cod_data_source_block           cu_r22c6_0m
_cod_database_code               4124190
_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.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C13(H13A,H13B), C1(H1A,H1B), C12(H12A,H12B),
 C21(H21A,H21B), C24(H24A,H24B)
2.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), N1(H1), C15(H15), C17(H17), C19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'