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_1511944
_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_sum            'C213 H24 O12'
_chemical_formula_weight         2774.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -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                   23.187(3)
_cell_length_b                   23.187(3)
_cell_length_c                   26.056(5)
_cell_measurement_temperature    100
_cell_volume                     14009(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ADSC-Q315 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  0.0811
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54405
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         0.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5592
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.137
_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   2.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         17014
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      2.229
_refine_ls_R_factor_all          0.2171
_refine_ls_R_factor_gt           0.2016
_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          0.4817
_refine_ls_wR_factor_ref         0.5027
_reflns_number_gt                14100
_reflns_number_total             17014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4006882_si_005.cif
_cod_data_source_block           12B01dan02
_cod_original_sg_symbol_H-M      P-4
_cod_database_code               1511944