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_4025058
_publ_contact_author_address
;
     The University of Arizona
     Department of Chemistry and Biochemistry
     1306 E. University Boulevard
     Tucson, AZ 85721-0041
     USA
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_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
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Synthesis of Conformationally Constrained Diaminodicarboxylic Acid
Derivatives
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_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         '(C11 H20 N2 O4), Cl2'
_chemical_formula_sum            'C11 H20 Cl2 N2 O4'
_chemical_formula_weight         315.19
_chemical_name_common            'spirobisaminoester HCl salt'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.511(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.681(6)
_cell_length_b                   16.982(12)
_cell_length_c                   11.343(8)
_cell_measurement_reflns_used    400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.18
_cell_measurement_theta_min      2.40
_cell_volume                     1672(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.2568
_diffrn_reflns_av_sigmaI/netI    0.3166
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4215
_diffrn_reflns_theta_full        18.85
_diffrn_reflns_theta_max         18.85
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.28
_diffrn_standards_interval_time  2520
_diffrn_standards_number         7
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9960
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0047(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1307
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.778
_refine_ls_R_factor_all          0.2342
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                395
_reflns_number_total             1307
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jo901892d_si_002_1.cif
_cod_data_source_block           15
_cod_depositor_comments
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The following automatic conversions were performed:
data name '_symmetry_space_group_it_number' replaced with
'_space_group_IT_number' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

'_symmetry_space_group_number'
data item was removed -- it should have been renamed to
'_space_group_IT_number' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4025058