Preparation of Tris(spiroorthocarbonate) Cyclophanes as Back to Back Ditopic Hosts
Danjo, Hiroshi; Iwaso, Kazuhisa; Kawahata, Masatoshi; Ohara, Kazuaki; Miyazawa, Toshifumi; Yamaguchi, Kentaro; Organic Letters 15 (2013) 2164–; doi:10.1021/ol4006882

data_1511943
_publ_section_title
;
 Preparation of Tris(spiroorthocarbonate) Cyclophanes as Back to Back
 Ditopic Hosts
;
_journal_issue                   9
_journal_name_full               'Organic Letters'
_journal_page_first              2164
_journal_paper_doi               10.1021/ol4006882
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         C87H78O12,2(C60)
_chemical_formula_sum            'C207 H78 O12'
_chemical_formula_weight         2756.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.459(3)
_cell_length_b                   22.459(3)
_cell_length_c                   25.656(5)
_cell_measurement_temperature    100
_cell_volume                     12941(4)
_computing_cell_refinement       'HKL 2000'
_computing_data_collection       'HKL 2000'
_computing_data_reduction        'HKL 2000'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 19.4932
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'ADSC-Q210 CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75000
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3937
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5664
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       0.0062(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0776
_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 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                3868
_reflns_number_total             3937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4006882_si_004.cif
_cod_data_source_block           12B01dan05
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               1511943