Planar chiral asymmetric naphthalenediimide cyclophanes: synthesis, characterization and tunable FRET properties
Gabutti, Sandro; Schaffner, Silvia; Neuburger, Markus; Fischer, Matthias; Schäfer, Gabriel; Mayor, Marcel; Organic & Biomolecular Chemistry 7 (2009) 3222–3229; doi:10.1039/b905945h

data_7150693
_publ_section_title
;
 Planar chiral asymmetric naphthalenediimide cyclophanes: synthesis,
 characterization and tunable FRET properties
;
_journal_issue                   16
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              3222
_journal_page_last               3229
_journal_paper_doi               10.1039/b905945h
_journal_volume                  7
_journal_year                    2009
_chemical_formula_moiety         'C60 H56 N4 O8 S2, C4 H8 O2'
_chemical_formula_sum            'C64 H64 N4 O10 S2'
_chemical_formula_weight         1113.37
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4787(5)
_cell_length_b                   23.2471(6)
_cell_length_c                   31.7802(9)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    123
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     11435.6(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            106563
_diffrn_reflns_theta_full        26.438
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         2.035
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0525
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         9267
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.000970
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.297 0.336 0.111
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1278
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0661
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                9875
_reflns_number_total             11720
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      1219.61
_oxford_refine_ls_r_factor_ref   0.0697
_oxford_refine_ls_scale          0.03186(5)
_oxford_reflns_number_all        11685
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b905945h.txt
_cod_data_source_block           sg_cyclS2_last
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               7150693