Preparation, solid-state characterization, and computational study of a crown ether attached to a squaramide.
Frontera, Antonio; Orell, Maria; Garau, Carolina; Quiñonero, David; Molins, Elies; Mata, Ignasi; Morey, Jeroni; Organic letters 7 (2005) 1437–1440; doi:10.1021/ol0474608

data_1506457
_publ_section_title
;
 Preparation, solid-state characterization, and computational study of a
 crown ether attached to a squaramide.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1437
_journal_page_last               1440
_journal_paper_doi               10.1021/ol0474608
_journal_volume                  7
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H38 N2 O8'
_chemical_formula_structural     'C32 H38 N2 O8'
_chemical_formula_sum            'C32 H38 N2 O8'
_chemical_formula_weight         578.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-07-30T12:44:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                83.18
_cell_angle_beta                 70.88
_cell_angle_gamma                78.91
_cell_formula_units_Z            2
_cell_length_a                   10.373
_cell_length_b                   10.925
_cell_length_c                   14.066
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1475.296
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.9186E-2
_diffrn_orient_matrix_UB_12      0.93109E-1
_diffrn_orient_matrix_UB_13      -0.9418E-2
_diffrn_orient_matrix_UB_21      0.20706E-1
_diffrn_orient_matrix_UB_22      -0.5272E-2
_diffrn_orient_matrix_UB_23      -0.74186E-1
_diffrn_orient_matrix_UB_31      -0.100737
_diffrn_orient_matrix_UB_32      0.6049E-2
_diffrn_orient_matrix_UB_33      0.9617E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.2042
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6281
_diffrn_reflns_theta_full        26.24
_diffrn_reflns_theta_max         26.24
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 81
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.8263
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   7
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.2549
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0722P)2^+0.0044P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                2051
_reflns_number_total             5936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0474608si20041210_052554.cif
_cod_data_source_block           pm55
_cod_original_cell_volume        1475.3
_cod_database_code               1506457
_exptl_absorpt_factor_mur        0.008
_exptl_absorpt_correction_t_ave  0.9011
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1