A molecular shuttle that operates inside a metal-organic framework
Kelong Zhu; Christopher A. O'Keefe; V. Nicholas Vukotic; Robert W. Schurko; Stephen J. Loeb; Nature Chemistry 7 (2015) 514–519; doi:10.1038/nchem.2258

data_1520105
_publ_section_title
;
 A molecular shuttle that operates inside a metal-organic framework
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              514
_journal_page_last               519
_journal_paper_doi               10.1038/nchem.2258
_journal_volume                  7
_journal_year                    2015
_chemical_formula_moiety         'C52 H38 N4 O8, C16 H32 O8, C4 H10 O2'
_chemical_formula_sum            'C72 H80 N4 O18'
_chemical_formula_weight         1289.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                106.0735(15)
_cell_angle_beta                 101.0732(16)
_cell_angle_gamma                92.4060(16)
_cell_formula_units_Z            2
_cell_length_a                   12.6007(4)
_cell_length_b                   16.0006(5)
_cell_length_c                   17.3353(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3279.14(18)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48851
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         2.714
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         10914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1018P)^2^+4.6836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7653
_reflns_number_total             10914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2258-s2.cif
_cod_data_source_block           MIM_LINKER_4
_cod_database_code               1520105
_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:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B), C66(H66A,H66B), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C13(H13), C14(H14), C16(H16),
 C17(H17), C19(H19), C20(H20), C25(H25), C26(H26), C28(H28), C29(H29), C34(H34),
  C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C46(H46), C47(H47),
 C49(H49), C50(H50)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C52(H52A,H52B,
 H52C), C1C(H1CA,H1CB,H1CC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              92646
_shelx_hkl_checksum              79844