Squaraine-Derived Rotaxanes: Sterically Protected Fluorescent Near-IR Dyes
Easwaran Arunkumar; Christopher C. Forbes; Bruce C. Noll; Bradley D. Smith; Journal of the American Chemical Society 127 (2005) 3288–3289; doi:10.1021/ja042404n

data_4111505
_publ_contact_author_address
;Department of Chemistry and Biochemistry
University of Notre Dame
Notre Dame, IN 46556
USA
;
_publ_contact_author_email       Bradley.D.Smith.115@nd.edu
_publ_contact_author_fax         01(574)6316652
_publ_contact_author_name        'Professor Bradley D. Smith'
_publ_contact_author_phone       01(574)6318632
_publ_section_title
;
 Squaraine-Derived Rotaxanes: Sterically Protected Fluorescent Near-IR
 Dyes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3288
_journal_page_last               3289
_journal_paper_doi               10.1021/ja042404n
_journal_volume                  127
_journal_year                    2005
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C44 H36 N2 O2, C30 H26 N6 O4, 2(H2 O)'
_chemical_formula_sum            'C74 H66 N8 O8'
_chemical_formula_weight         1195.35
_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                86.839(1)
_cell_angle_beta                 78.258(1)
_cell_angle_gamma                77.305(1)
_cell_formula_units_Z            1
_cell_length_a                   9.7987(1)
_cell_length_b                   10.9613(2)
_cell_length_c                   14.4900(2)
_cell_measurement_reflns_used    6017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.434
_cell_measurement_theta_min      2.358
_cell_volume                     1486.41(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38334
_diffrn_reflns_theta_full        31.54
_diffrn_reflns_theta_max         31.54
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.'
_exptl_crystal_colour            'translucent blue'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       needle
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         9802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0598P)^2^+0.4764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                8035
_reflns_number_total             9802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042404nsi20041217_114824.cif
_cod_data_source_block           bcn148_0m
_cod_database_code               4111505