Dipeptide Surrogates Containing Asparagine-Derived Tetrahydropyrimidinones: Preparation, Structure, and Use in Solid Phase Synthesis
Joseph P. Konopelski; Lubov K. Filonova; Marilyn M. Olmstead; Journal of the American Chemical Society 119 (1997) 4305–4306; doi:10.1021/ja9639271

data_4116965
_publ_section_title
;
 Dipeptide Surrogates Containing Asparagine-Derived
 Tetrahydropyrimidinones: Preparation, Structure, and Use in Solid Phase
 Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4305
_journal_page_last               4306
_journal_paper_doi               10.1021/ja9639271
_journal_volume                  119
_journal_year                    1997
_chemical_formula_moiety         ' C9 H15 Rh1 N1 P2 F12 Cl1 '
_chemical_formula_sum            'C9 H15 Cl F12 N P2 Rh'
_chemical_formula_weight         674.7
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                76.39(2)
_cell_angle_beta                 82.31(2)
_cell_angle_gamma                87.26(2)
_cell_formula_units_Z            1
_cell_length_a                   6.617(2)
_cell_length_b                   7.436(2)
_cell_length_c                   13.965(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      13.0
_cell_volume                     661.7(3)
_computing_cell_refinement       'CAD-4 EXPRESS software (Enraf-Nonius)'
_computing_data_collection       'CAD-4 EXPRESS software (Enraf-Nonius)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      293
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            2476
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        3.39
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.43
_exptl_absorpt_correction_T_max  1.08
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            ' yellow '
_exptl_crystal_description       ' Parallelepiped '
_exptl_crystal_F_000             315.2
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.921
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.6013
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         2191
_refine_ls_R_factor_obs          0.0440
_refine_ls_shift/esd_max         1.4747
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0484
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              9
_reflns_limit_k_min              -8
_reflns_limit_l_max              17
_reflns_limit_l_min              1
_reflns_number_observed          2191
_reflns_number_total             2476
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ja9639271_1.cif
_cod_data_source_block           C9H15Rh1N1P2F12Cl1
_cod_depositor_comments
;
 Removing the _exptl_crystal_density_diffrn data item since it clearly
 contains an incorrect value ("0.0").

 Antanas Vaitkus,
 2018-07-17

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        661.8(3)
_cod_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum        ' C9 H15 Rh1 N1 P2 F12 Cl1 '
_cod_database_code               4116965