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_4124191
_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         '0.25(C496 H472 Cu48 N64 O240)'
_chemical_formula_sum            'C123 H199 Cu6 N27 O50'
_chemical_formula_weight         3237.32
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1284(6)
_cell_length_b                   26.1284(6)
_cell_length_c                   34.1663(9)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.093
_cell_measurement_theta_min      3.523
_cell_volume                     23325.1(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.94
_diffrn_measured_fraction_theta_full 0.791
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_laue_measured_fraction_full 0.791
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53898
_diffrn_reflns_point_group_measured_fraction_full 0.791
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.913
_diffrn_reflns_theta_min         2.391
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.8430.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    0.922
_exptl_crystal_F_000             6800
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8519
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1035P)^2^+149.1925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8155
_reflns_number_total             8519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04674_si_004.cif
_cod_data_source_block           cu_nv003_0m_sqd
_cod_original_cell_volume        23325.1(12)
_cod_database_code               4124191
_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, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1S \\sim N1S \\sim C1S \\sim C2S \\sim C3S: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O2S \\sim N2S \\sim C4S \\sim C5S \\sim C6S: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: O3W(0.5) H3WA(0.5)
4.a Riding coordinates:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
4.c Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC)
4.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C5(H5), C7(H7), C11(H11), C13(H13), C15(H15), C20(H20),
 C22(H22), C24(H24), C1S(H1S), O2S(H2S), C4S(H4S)
;
_olex2_submission_special_instructions 'No special instructions were received'