The "Azido Gauche Effect" Implications for the Conformation of Azidoprolines
Louis-Sebastian Sonntag; Sabine Schweizer; Christian Ochsenfeld; Helma Wennemers; Journal of the American Chemical Society 128 (2006) 14697–14703; doi:10.1021/ja0654938

data_4111069
_publ_contact_author_address
; Chemical Crystallography Laboratory, 
 Department of Chemistry, 
 University of Oxford, 
 Chemistry Research Laboratory, 
 Mansfield Road, 
 Oxford, OX1 3TA, UK. 
;
_publ_contact_author_email       david.watkin@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285018'
_publ_contact_author_name        'David Watkin'
_publ_contact_author_phone       '+44 1865 285024'
_publ_section_title
;
 The "Azido Gauche Effect" Implications for the Conformation of
 Azidoprolines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14697
_journal_page_last               14703
_journal_paper_doi               10.1021/ja0654938
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H12 N4 O3'
_chemical_formula_sum            'C8 H12 N4 O3'
_chemical_formula_weight         212.21
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-01-26
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 115.0156(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2443(2)
_cell_length_b                   12.7360(2)
_cell_length_c                   9.4877(2)
_cell_measurement_reflns_used    4700
_cell_measurement_temperature    173
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1
_cell_volume                     1012.25(4)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7874
_diffrn_reflns_theta_full        27.870
_diffrn_reflns_theta_max         27.870
_diffrn_reflns_theta_min         2.369
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9367
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000232
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.268 0.155 0.726E-01 -0.317E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0495
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0397
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2226
_reflns_number_total             2524
_reflns_threshold_expression     I>0.50u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.4114(8)
_oxford_structure_analysis_title '1261253 lsd429_173k'
_cod_data_source_file            ja0654938si20060730_075708.cif
_cod_data_source_block           lsd429
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4111069