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_4037876
_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            'C52 H74 O6'
_chemical_formula_weight         795.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.301(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8429(16)
_cell_length_b                   15.1141(15)
_cell_length_c                   9.6013(10)
_cell_measurement_reflns_used    97
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.8860
_cell_measurement_theta_min      2.6731
_cell_volume                     2289.2(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.1586
_diffrn_reflns_av_unetI/netI     0.1666
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            44832
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         2.521
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 1382 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.639
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7698
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.638
_refine_ls_R_factor_all          0.2594
_refine_ls_R_factor_gt           0.1643
_refine_ls_shift/su_max          2.767
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2888
_refine_ls_wR_factor_ref         0.3261
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                4329
_reflns_number_total             7698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03030_si_002.cif
_cod_data_source_block           JvM_LS_rotaxaan_0ma_a
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4037876
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41997
_shelx_hkl_checksum              99962