Synthesis of fluorescent stilbene and tolan rotaxanes by Suzuki coupling
Stanier, Carol A.; O’Connell, Michael J.; Anderson, Harry L.; Clegg, William; Chemical Communications  (2001) 493–; doi:10.1039/b010015n

data_7114919
_publ_section_title
;
 Synthesis of fluorescent stilbene and tolan rotaxanes by Suzuki coupling
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              493
_journal_paper_doi               10.1039/b010015n
_journal_year                    2001
_chemical_formula_sum            'C66 H80 O38'
_chemical_formula_weight         1481.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.479(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.767(5)
_cell_length_b                   13.960(3)
_cell_length_c                   28.085(7)
_cell_measurement_reflns_used    22609
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      2.39
_cell_volume                     7766(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69420
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19962
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     1354
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1680
_refine_ls_R_factor_gt           0.1638
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1542P)^2^+272.7736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3911
_refine_ls_wR_factor_ref         0.3941
_reflns_number_gt                9681
_reflns_number_total             10443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b010015n.txt
_cod_data_source_block           oxdp4
_cod_original_sg_symbol_H-M      I2
_cod_database_code               7114919