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_7109337
_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_formula_moiety
'C39 H40 N4 O4, 2(C32 H28 N4 O4), 3.5(C2 H6 O)'
_chemical_formula_sum            'C110 H117 N12 O15.5'
_chemical_formula_weight         1855.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.488(8)
_cell_angle_beta                 97.325(7)
_cell_angle_gamma                97.504(7)
_cell_formula_units_Z            2
_cell_length_a                   10.8101(6)
_cell_length_b                   21.2231(13)
_cell_length_c                   22.7870(16)
_cell_measurement_reflns_used    21641
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      3.0
_cell_volume                     4770.1(6)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33613
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1970
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1316
_refine_ls_number_reflns         16656
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0816
_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
[0.00000+1.00000exp(0.26(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+2.8765*P+(0.0991P)^2^+0.0000sin\q/\l]
where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2292
_reflns_number_gt                9224
_reflns_number_total             16656
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc42045k.txt
_cod_data_source_block           '[3]rotaxane_9'
_cod_original_cell_volume        4770.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C110 H117 N12 O15.50'
_cod_database_code               7109337