A covalent and modular synthesis of homo and hetero [n]rotaxanes.
Cornelissen, Milo D.; Pilon, Simone; Steemers, Luuk; Wanner, Martin J.; Frölke, Steven; Zuidinga, Ed; Jorgensen, Steen Ingemann; van der Vlugt, Jarl Ivar; van Maarseveen, Jan H.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03030

data_4037877
_publ_section_title
;
 A covalent and modular synthesis of homo and hetero [n]rotaxanes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03030
_journal_year                    2020
_chemical_formula_sum            'C25 H38 N3 O3'
_chemical_formula_weight         428.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                105.542(6)
_cell_angle_beta                 94.855(6)
_cell_angle_gamma                96.174(6)
_cell_formula_units_Z            2
_cell_length_a                   8.7409(19)
_cell_length_b                   12.748(3)
_cell_length_c                   13.057(3)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4195
_cell_measurement_theta_min      2.7014
_cell_volume                     1383.8(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.923
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31005
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.301
_diffrn_reflns_theta_min         2.643
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.755
_exptl_crystal_size_mid          0.620
_exptl_crystal_size_min          0.288
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.084
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.1547
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3741
_refine_ls_wR_factor_ref         0.4082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3596
_reflns_number_total             4634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03030_si_003.cif
_cod_data_source_block           JvM_SP_rotzax_thread_N3_0m_a
_cod_database_code               4037877
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              74433
_shelx_hkl_checksum              25303