Squaraine Rotaxanes with Boat Conformation Macrocycles
Na Fu; Jeffrey M. Baumes; Easwaran Arunkumar; Bruce C. Noll; Bradley D. Smith; Journal of Organic Chemistry 74 (2009) 6462–6468; doi:10.1021/jo901298n

data_4024825
_publ_section_title
;
Squaraine Rotaxanes with Boat Conformation Macrocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6462
_journal_page_last               6468
_journal_paper_doi               10.1021/jo901298n
_journal_volume                  74
_journal_year                    2009
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C74 H58 N8 O6 I4, C H Cl3, C6 H14'
_chemical_formula_sum            'C81 H73 Cl3 I4 N8 O6'
_chemical_formula_weight         1868.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                86.541(3)
_cell_angle_beta                 82.282(3)
_cell_angle_gamma                82.283(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2502(7)
_cell_length_b                   16.0849(8)
_cell_length_c                   17.9953(10)
_cell_measurement_reflns_used    7234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.1734
_cell_measurement_theta_min      2.3367
_cell_volume                     3762.6(3)
_computing_cell_refinement       'Apex2 (Bruker, 2004)'
_computing_data_collection       'Apex2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 2001)'
_computing_publication_material  'enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-ApexII CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63848
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2004). SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            'blue green'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_platon_squeeze_details          ' ?'
_refine_diff_density_max         4.747
_refine_diff_density_min         -4.404
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         13265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+39.8820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                9458
_reflns_number_total             13265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901298n_si_002.cif
_cod_data_source_block           bcn258_1sq
_cod_database_code               4024825