A New Class of Intramolecularly Hydrogen-Bonded Dendrons Based on a 2-Methoxyisophthalamide Repeat Unit
Christopher J. Gabriel; Matthew P. DeMatteo; Noel M. Paul; Tomohisa Takaya; Terry L. Gustafson; Christopher M. Hadad; Jon R. Parquette; Journal of Organic Chemistry 71 (2006) 9035–9044; doi:10.1021/jo061351k

data_4022095
_publ_section_title
;
 A New Class of Intramolecularly Hydrogen-Bonded Dendrons
 Based on a 2-Methoxyisophthalamide Repeat Unit
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9035
_journal_page_last               9044
_journal_paper_doi               10.1021/jo061351k
_journal_volume                  71
_journal_year                    2006
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H35 N3 O9'
_chemical_formula_sum            'C31 H35 N3 O9'
_chemical_formula_weight         593.62
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-09-27T11:08:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.059(6)
_cell_angle_beta                 112.550(6)
_cell_angle_gamma                92.755(6)
_cell_formula_units_Z            2
_cell_length_a                   10.870(2)
_cell_length_b                   11.836(2)
_cell_length_c                   13.685(2)
_cell_measurement_reflns_used    5440
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     1557.6(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.244616E-1
_diffrn_orient_matrix_UB_12      -0.688518E-1
_diffrn_orient_matrix_UB_13      -0.438127E-1
_diffrn_orient_matrix_UB_21      0.768132E-1
_diffrn_orient_matrix_UB_22      0.527701E-1
_diffrn_orient_matrix_UB_23      0.30099E-2
_diffrn_orient_matrix_UB_31      0.606293E-1
_diffrn_orient_matrix_UB_32      -0.159444E-1
_diffrn_orient_matrix_UB_33      0.698455E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29451
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+0.1850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                4308
_reflns_number_total             5491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061351ksi20060705_035807.cif
_cod_database_code               4022095