Investigation of conjugate addition/intramolecular nitrone dipolar cycloadditions and their use in the synthesis of dendrobatid alkaloid precursors.
Horsley, Helen T.; Holmes, Andrew B.; Davies, John E.; Goodman, Jonathan M.; Silva, María A; Pascu, Sofia I.; Collins, Ian; Organic & biomolecular chemistry 2 (2004) 1258–1265; doi:10.1039/b402307b

data_7150377
_publ_section_title
;
 Investigation of conjugate addition/intramolecular nitrone dipolar
 cycloadditions and their use in the synthesis of dendrobatid alkaloid
 precursors.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1258
_journal_page_last               1265
_journal_paper_doi               10.1039/b402307b
_journal_volume                  2
_journal_year                    2004
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C13 H17 N3 O1 '
_chemical_formula_sum            'C13 H17 N3 O'
_chemical_formula_weight         231.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-20-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 107.01(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.610(3)
_cell_length_b                   12.464(3)
_cell_length_c                   16.763(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    240
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      5.10
_cell_volume                     2519.4(10)
_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 (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      240
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21461
_diffrn_reflns_theta_full        25.804
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         5.123
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            ' white '
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             992.000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1747
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000186
_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:
1.76 1.51 1.44
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0581
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0443
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2637
_reflns_number_total             5684
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            b402307b.txt
_cod_data_source_block           ah0320_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        2519.5(10)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C13 H17 N3 O1 '
_cod_database_code               7150377