Phthalocrowns: Isoindoline-Crown Ether Macrocycles
Ingrid-Suzy Tamgho; James T. Engle; Christopher J. Ziegler; Journal of Organic Chemistry 77 (2012) 11372–11376; doi:10.1021/jo302227z

data_4027792
_publ_section_title
;
 Phthalocrowns: Isoindoline-Crown Ether Macrocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11372
_journal_page_last               11376
_journal_paper_doi               10.1021/jo302227z
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C14 H17 N3 O2'
_chemical_formula_weight         259.31
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.9063(3)
_cell_length_b                   10.3310(3)
_cell_length_c                   13.8954(4)
_cell_measurement_reflns_used    4661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.42
_cell_measurement_theta_min      4.97
_cell_volume                     1278.53(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4825
_diffrn_reflns_theta_full        66.42
_diffrn_reflns_theta_max         66.42
_diffrn_reflns_theta_min         5.34
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.8819
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; [Sheldrick, G. M. (2004)]'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0564P)^2^+0.1964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                2030
_reflns_number_total             2046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302227z_si_003.cif
_cod_data_source_block           3_orthorhombic
_cod_database_code               4027792