Synthesis of Conformationally Constrained Diaminodicarboxylic Acid Derivatives
Robin A. Weatherhead; Michael D. Carducci; Eugene A. Mash; Journal of Organic Chemistry 74 (2009) 8773–8778; doi:10.1021/jo901892d

data_4025061
_publ_contact_author_address
;
     The University of Arizona
     Department of Chemistry and Biochemistry
     1306 E. University Boulevard
     Tucson, AZ 85721-0041
     USA
;
_publ_contact_author_email       emash@u.arizona.edu
_publ_contact_author_fax         520-621-8407
_publ_contact_author_name        'Professor Eugene A. Mash, Jr.'
_publ_contact_author_phone       520-621-6321
_publ_section_title
;
Synthesis of Conformationally Constrained Diaminodicarboxylic Acid
Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8773
_journal_page_last               8778
_journal_paper_doi               10.1021/jo901892d
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C34 H36 N2 O8'
_chemical_formula_sum            'C34 H36 N2 O8'
_chemical_formula_weight         600.65
_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_creation_method           SHELXL-97
_cell_angle_alpha                98.037(2)
_cell_angle_beta                 106.442(2)
_cell_angle_gamma                100.826(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7824(8)
_cell_length_b                   9.1091(9)
_cell_length_c                   11.1134(11)
_cell_measurement_reflns_used    2822
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.249
_cell_measurement_theta_min      2.3255
_cell_volume                     726.43(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8288
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        .32
_diffrn_standards_interval_count 3636
_diffrn_standards_number         19
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.899488
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Bruker 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                1822
_reflns_number_total             2981
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jo901892d_si_002_4.cif
_cod_data_source_block           25
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4025061