Synthesis of fumaramide derived [3]rotaxanes as potential precursors for molecular boxes
Nigel S. Simpkins; Damian F. Weske; Louise Male; Simon J. Coles; Mateusz B. Pitak; Chem.Commun. 49 (2013) 5010–; doi:10.1039/c3cc42045k

data_7109338
_publ_section_title
;
 Synthesis of fumaramide derived [3]rotaxanes as potential precursors for
 molecular boxes
;
_journal_name_full               Chem.Commun.
_journal_page_first              5010
_journal_paper_doi               10.1039/c3cc42045k
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C37 H36 N4 O4, 2(C32 H28 N4 O4), 0.5(C2 H6 O), 0.5(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C102.5 H101 N12 O15'
_chemical_formula_weight         1740.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.610(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0536(3)
_cell_length_b                   38.7489(11)
_cell_length_c                   11.7046(3)
_cell_measurement_reflns_used    7785
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.820
_cell_measurement_theta_min      3.781
_cell_volume                     4555.0(2)
_computing_cell_refinement       'SAINT V6.28A (Bruker, 1997)'
_computing_data_collection       'SMART V5.626 (Bruker, 1997)'
_computing_data_reduction        'SAINT V6.28A (Bruker, 1997)'
_computing_molecular_graphics
;
OLEX2 (Dolomanov, O.V., Bourhis, L.J., Gildea, R.J., Howard, J.A.K,
& Puschmann, H., 2009)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
Sir2004 (Burla, Caliandro, Camalli, Carrozzini, Cascarano,
De Caro, Giacovazzo, Polidori, & Spagna, 2005)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27608
_diffrn_reflns_theta_full        66.58
_diffrn_reflns_theta_max         66.58
_diffrn_reflns_theta_min         6.35
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.8671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.07 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Slab
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1191
_refine_ls_number_reflns         13650
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+1.0238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                12562
_reflns_number_total             13650
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc42045k.txt
_cod_data_source_block           '[3]rotaxane_10'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C102.50 H101 N12 O15'
_cod_database_code               7109338